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GB/T 9725-2007 | English | 209 |
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Chemical reagent -- General rule for potentiometric titration
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GB/T 9725-1988 | English | 279 |
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Chemical reagent--General rules for potentiometric titration
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PDF similar to GB/T 9725-2007
Basic data Standard ID | GB/T 9725-2007 (GB/T9725-2007) | Description (Translated English) | Chemical reagent -- General rule for potentiometric titration | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | G60 | Classification of International Standard | 71.040.30 | Word Count Estimation | 8,878 | Date of Issue | 2007-09-26 | Date of Implementation | 2008-04-01 | Older Standard (superseded by this standard) | GB/T 9725-1988 | Quoted Standard | GB/T 601; GB/T 6682 | Adopted Standard | ISO 6353-1-1982, NEQ | Regulation (derived from) | China National Standard Approval Announcement2007 No.11 (Total No.111) | 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 the titration endpoint is determined by measuring the electrode potential methods. This standard applies to acid-base titration, precipitation titration, redox titration and non- aqueous titration. Especially for turbidity, colored solution titration method analysis and titration of the lack of a suitable indicator. |
GB/T 9725-2007: Chemical reagent -- General rule for potentiometric titration---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.
Chemical reagent. General rule for potentiometric titration
ICS 71.040.30
G60
National Standards of People's Republic of China
Replacing GB/T 9725-1988
Chemical reagent potentiometric titration method
(ISO 6353-1. 1982, Reagents for chemical micro analysis-
Part 1. Generaltestmethods, NEQ)
2007-09-26 released
2008-04-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
China National Standardization Administration released
Foreword
This standard and ISO 6353-1. 1982 "Chemical Analysis Reagents Part 1. Common test methods" consistency is not equivalent.
This standard replaces GB/T 9725-1988 "chemical reagent potentiometric titration method", compared with GB/T 9725-1988 main changes
as follows.
--- Modify the principle of the method (see Chapter 3);
--- Improve the accuracy of the instrument (1988 version of 5.2, this version of 5.2,5.3);
--- Increased composite electrode (version 5.4);
--- Elimination of antimony electrodes and tungsten electrodes (1988 edition of 5.3.1.2,5.3.2.3);
--- Modify the schematic diagram of the instrument (1988 version 6.1, version 5.1);
--- Modify the contents of Appendix A (see Appendix A);
--- Canceled Appendix B, Appendix C (1988 edition of Appendix B, Appendix C).
Appendix A of this standard is an informative annex.
This standard is proposed by China Petroleum and Chemical Industry Association.
This standard by the National Standardization Technical Committee Chemical Reagent Branch (SAC/TC63/SC3) centralized.
This standard was drafted. Guangzhou Chemical Reagent Factory.
The main drafters of this standard. Yu Qi, Liu Zhao Yuan, Fu Qionglian.
This standard was first released in 1977, the first revision in 1988.
Chemical reagent potentiometric titration method
1 Scope
This standard specifies the method by measuring the electrode potential to determine the end point of titration.
This standard applies to acid-base titration, sedimentation titration, redox titration and non-titration. Particularly suitable for turbid, colored solution titration
And titration analysis methods that lack suitable indicators.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. All dated references, which are subsequently owned
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to reach an agreement based on this standard research
Whether you can use the latest versions of these files. For undated references, the latest version applies to this standard.
GB/T 601 chemical reagent standard titration solution preparation
GB/T 6682 analytical laboratory water specifications and test methods (GB/T 6682-1992, neq ISO 3696. 1987)
3 method principle
The specified instruction electrode and reference electrode immersed in the same solution under test, the titration process, the reference electrode potential remains constant, the fingers
The potential of the electrode changes with the concentration of the tested substance. Before and after the stoichiometry, the concentration of the measured substance in the solution changes, can cause
Steep changes in the electrode potential indicate that the sudden change in the electrode potential is the end point of the titration.
4 Reagents and materials
The standard titration solution used in this standard prepared according to GB/T 601 regulations, the experimental water should be consistent with the three water GB/T 6682
specification.
5 instruments and devices
5.1 Potentiometric titration device
Potentiometric titration device shown in Figure 1.
5.2 Potentiometer
Potentiometer accuracy of ± 2mV.
5.3 acidity meter
The accuracy of pH meter is ± 0.02.
5.4 Electrode
See Appendix A for electrode selection.
This standard specifies.
a) glass electrode for indicating electrode, silver electrode and platinum electrode;
b) saturated calomel electrode for reference electrode, double salt bridge saturated calomel electrode;
c) Composite electrode.
5.5 electromagnetic stirrer
1 --- Burette;
2 --- indicating electrode;
3 --- reference electrode;
4 --- beaker
5 --- test solution;
6 --- electromagnetic stirrer;
7 --- potentiometer or pH meter;
8 --- display window.
Figure 1 potentiometric titration device
6 assay
6.1 Determination methods
Sampling according to the provisions of the product standards and preparation of test solution. Insert the specified electrode, start the electromagnetic stirrer, with the provisions of the standard titration solution into
Line titration. From the burette, a standard titration solution of about 90% of the desired titration volume is added and the potential or pH of the solution is measured.
After each drop plus 1mL or standard titration solution to measure a potential or pH, before and after the stoichiometry, 0.1mL per drop should be added
Quasi-titration solution, measured once. Continue to titrate until the potential or pH changes little. Record each drop after dropping standard titration solution
The tube readings and measured potentials or pH values are used as a plot or second-order derivative to determine the titration endpoint.
6.2 Determination of the end point
6.2.1 Mapping method
The titration curve is plotted using the mV or pH of the indicator electrode as the ordinate and the reading of the burette (mL) as the abscissa. Do two
And the abscissa 45 ° titration curve tangential line, and in the two tangent line with a tangent distance equal to the parallel line, the line with the titration curve
The intersection point is the titration end point (see Figure 2). The abscissa of intersection point is the dosage of standard titration solution when titration end point, and the ordinate of intersection point is drop
Set the end of the potential or pH.
1 --- titration curve;
2 --- tangent
3 --- parallel equidistance line;
4 --- titration end.
Figure 2 titration end point curve
6.2.2 second-level micro-business law
Buret reading 犞 (mL) and the corresponding potential E (mV) or pH are tabulated and the following values calculated.
The volume of standard titration solution is applied dropwise (Δ 犞).
Changes in potential or pH (ΔE or ΔpH) each time a standard titration solution is dropped.
A level of micro-value. That is, the change of potential or pH value caused by standard titration solution per unit volume is equal to ΔE/Δ 犞 or
ΔpH/Δ 犞.
Second-level derivative. Numerically equal to the difference between adjacent first derivative.
First derivative, the second derivative is equal to zero when titration end.
The volume of the standard titration solution titration end point to 犞 0, the value expressed in milliliters (mL), according to equation (1) Calculated.
犞 0 = 犞 + 犪 犪 - 犫 × Δ () 犞 (1)
Where.
犞 --- second derivative for the volume when the standard titration solution, in milliliters (mL);
犪 --- second derivative before the two micro-value;
犫 --- second derivative after two micro-value;
Δ 犞 --- from the second derivative to 犪 to second derivative for 犫 when the volume of the standard titration solution, in milliliters (mL).
An example of a second-level micro-business method for determining the end point is shown in Table 1.
Table 1 two micro-business law to determine the end of the instance
犞 /
mL
E /
mV
ΔE /
mV
Δ 犞 /
mL
A micro-business
(ΔE/Δ 犞)
Second-level micro-business
33.00 405
33.40 415
33.60 422
33.80 431
34.00 443
34.10 455
34.20 470
34.30 514
34.40 569
34.50 588
34.60 599
34.70 606
10 0.40 25
7 0.20 35
9 0.20 45
12 0.30 60
12 0.10 120
15 0.10 150
44 0.10 440
55 0.10 550
19 0.10 190
11 0.10 110
7 0.10 70
-360
-80
-40
In Table 1, the maximum of the first derivative is 550, and the second derivative is the zero between 110 and -360. Checked from Table 1
犪 = 110, 犫 = -360, 犞 = 34.30 mL, Δ 犞 = 0.1 mL.
犞 0 = 34.30 mL + 110110 - (- 360) [] × 0.1 mL
= 34.30 mL + 0.02 mL
= 34.32 mL
Appendix A.
(Informative)
Electrode Selection Reference Table
Titration method
Electrode system
(Indication - reference)
Description
1. Aqueous Neutralization Glass - Saturated calomel
Composite electrode
(1) glass electrode. the new electrode should be soaked in water for more than 24h before use, standing after use
That is, cleaned and soaked in water.
(2) saturated calomel electrode. When using the upper electrode pin rubber plug must be pulled out to prevent
Only produce diffusion potential, affect the measurement results. Electrode potassium chloride solution can not be
There are air bubbles to prevent disconnection. The solution should be kept a little potassium chloride crystals to protect
Certificate of potassium chloride solution saturation. Note that the electrode liquid department is not stained or blocked, and
Ensure that the liquid part of the appropriate oozing flow rate.
(3) composite electrode. the use of the top of the electrode pin rubber plug must be pulled out to prevent production
Health diffusion potential, affect the measurement results. The external reference electrode of the electrode is potassium chloride
Solution (3mol/L), replenishment can be added from the top hole. No need to measure
When the electrode protection cap should be put on the cap should put a small amount of potassium chloride solution
(3mol/L), to keep the electrode bulb wet. Electrode Avoid prolonged immersion in the distillation
Water, protein solution and acidic fluoride solution and avoid with silicone grease
contact.
2. Redox platinum - saturated calomel platinum electrode. before use should pay attention to the electrode surface can not have oily substances, if necessary, acetone
Or chromic acid wash solution, then washed with water.
3. Silver volume method silver - saturated calomel (1) silver electrode. Before use, use a fine sandpaper to polish the surface, and then immersed in a small amount of nitric acid
Sodium dilute nitric acid (1 + 1) solution, until there is gas evolution until removed and washed with water
clean.
(2) double salt bridge saturated calomel electrode. salt bridge casing filled with saturated ammonium nitrate or potassium nitrate
Solution. Other considerations are the same as for saturated calomel electrodes.
4. Nonaqueous acidometric glass - saturated calomel
(Glacial acetic acid as solvent)
(1) glass electrode. usage and aqueous solution of the same.
(2) double salt bridge saturated calomel electrode. salt bridge casing saturated potassium chloride anhydrous B
Alcohol solution. Other considerations are the same as for saturated calomel electrodes.
5. Non-aqueous alkali Alkali glass - saturated calomel
(Alcohol or acetonitrile as solvent)
Glass electrode and double salt bridge saturated calomel electrode. usage and non-aqueous acid method the same.
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