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HG/T 3696.2-2011 English PDF (HGT3696.2-2011)

HG/T 3696.2-2011 English PDF (HGT3696.2-2011)

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HG/T 3696.2-2011: Inorganic chemicals for industrical use. Preparations of standard and reagent solutions for chemical analysis. Part 2: Preparations of standard solutions for impurity

This part specifies the preparation method of impurity standard solution for chemical analysis of inorganic chemical products. This part is applicable to the preparation of the standard solution of a certain element, ion or molecule of a precise amount in a certain volume as required for the determination of the impurity content in the inorganic chemical product analysis. It may also be used for chemical analysis of other chemical products.
HG/T 3696.2-2011
HG
CHEMICAL INDUSTRY STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
ICS 71.060.01;71.060.99
G 10
Registration number. 34582-2012
Replacing HG/T 3696.2-2002
Inorganic chemicals for industrial use - Preparations of
standard and reagent solutions for chemical analysis ?€?
Part 2. Preparations of standard solutions for impurity
ISSUED ON. DECEMBER 20, 2011
IMPLEMENTED ON. JULY 01, 2012
Issued by. Ministry of Industry and Information Technology of PRC
3. No action is required - Full-copy of this standard will be automatically and immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3
1 Scope ... 6
2 Normative references ... 6
3 General provisions ... 6
4 Warning ... 7
5 Preparation method ... 7
Appendix A (Informative) Calibration of sulfur impurity standard solution ... 19 Appendix B (Normative) Methods for determination of the content of two
solutions ... 20
Appendix C (Informative) Preparation method of impurity standard solution by organic molecules ... 22
Foreword
HG/T 3696 ?€?Inorganic chemicals for industrial use - Preparations of standard and reagent solutions for chemical analysis ?€? Part 2. Preparations of standard solutions for impurity?€? is divided into the following parts.
- Part 1. Preparations of standard volumetric solutions;
- Part 2. Preparations of standard solutions for impurity;
- Part 3. Preparation of reagent solutions.
This part is part 2 of HG/T 3696.
This part was drafted in accordance with the rules given in GB/T 1.1-2009. This part replaces HG/T 3696.2-2002 ?€?Inorganic chemicals for industrial use - Preparations of standard solutions for impurity for chemical analysis?€?. As compared with HG/T 3696.2-2002, the main technical changes of this part in addition to editorial changes are as follows.
- CHANGE the name of this part in accordance with the requirements of
GB/T 1.1-2009 into ?€?Inorganic chemicals for industrial use - Preparations of standard and reagent solutions for chemical analysis ?€? Part 2.
Preparations of standard solutions for impurity?€?;
- ADD the requirements for the required standard and reagent solutions
(SEE 3.3);
- ADD chapter 4 ?€?Warning?€? (SEE 4);
- MODIFY the name of Table 1 into ?€?Preparation of standard stock solution for metallic element impurity?€? (SEE 5.1; clause 4.1 of 2002 version);
- ADD the method of using high purity magnesium to prepare magnesium
impurity standard solution (SEE Table 1 of 5.1);
- ADD the method of using stannous chloride to prepare tin impurity
standard solution (SEE Table 1 of 5.1);
- DELETE the preparation of the ferrous impurity standard solutions (SEE Table 1 of 4.1 in 2002 version);
- MODIFY the name of Table 2 into ?€?Preparation of standard stock solution of non-metallic element impurity?€? (SEE 5.2; 4.2 of 2002 version);
- ADD the preparation of standard solutions of iodine, fluorine and bromine in Table 2 as well as another preparation method of sulfur and chlorine impurity standard solutions (SEE Table 2 of 5.2);
Inorganic chemicals for industrial use - Preparations of
standard and reagent solutions for chemical analysis -
Part 2. Preparations of standard solutions for impurity
1 Scope
This part specifies the preparation method of impurity standard solution for chemical analysis of inorganic chemical products.
This part is applicable to the preparation of the standard solution of a certain element, ion or molecule of a precise amount in a certain volume as required for the determination of the impurity content in the inorganic chemical product analysis. It may also be used for chemical analysis of other chemical products. 2 Normative references
The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this Standard.
GB/T 6682-2008 Water for analytical laboratory use ?€? Specification and test methods
HG/T 3696.1 Inorganic chemicals for industrial use ?€? Preparations of
standard and reagent solutions for chemical analysis ?€? Part 1. Preparations of standard volumetric solutions
HG/T 3696.3 Inorganic chemicals for industrial use ?€? Preparations of
standard and reagent solutions for chemical analysis ?€? Part 3. Preparation of reagent solutions
3 General provisions
3.1 The water used in this part shall comply with the level III water requirements as specified in GB/T 6682-2008, unless otherwise specified.
3.2 The purity of the reagents used in this part shall be above analytical pure. The readily oxidized metal shall, before use, be subjected to surface treatment. 3.3 The standard and reagent solutions as required by the Appendixes of this part shall, unless otherwise specified, be prepared in accordance with the provisions of HG/T 3696.1 and HG/T 3696.3.
3.4 When diluting the impurity standard solution, it shall use accurate measuring device (pipette, volumetric flask) to perform integral multiple dilution. AND the volume of the standard solution measured each time shall be not less than 1.00 mL.
3.5 The standard solution for impurity determination shall, unless otherwise specified, be generally stored at room temperature for 12 months; AND it shall be prepared again when there is turbidity, precipitation, or color change. 3.6 The methods for the preparation of the impurity standard solutions as specified in this part are in alphabetical order.
3.7 The volume of the prepared stock solution in this part is for reference only; AND the user may adjust appropriately the preparation volume in accordance with the use amount, BUT it shall be at least not less than 100 mL.
4 Warning
Some of the reagents used in the preparation process of this part are toxic or corrosive, AND the operator must be careful! Any splashes on the skin must be flushed with water immediately, AND medical attention shall be
sought immediately if it is serious.
5 Preparation method
5.1 Preparation of standard solution of metallic element impurity
Unless otherwise specified, this impurity standard solution (SEE Table 1) shall be stored in a suitable plastic bottle.
Table 1 -- Preparation of standard stock solution of metallic element
impurity
Name Solution concentration Preparation method
Palladium
(Pd)
1 mL solution
contains 1 mg of
palladium (Pd)
WEIGH 0.833 g of palladium chloride which is dried in advance at
105 ??C ~ 110 ??C for 1 h; ADD 15 ml of 1 +4 hydrochloric acid
solution to dissolve it; TRANSFER all of it into a 500 ml volumetric
flask; DILUTE it to the mark; SHAKE to make it uniform.
Barium
(Ba)
1 mL solution
contains 1 mg of
barium (Ba)
1. WEIGH 0.889 g of barium chloride (BaCl2 ?€? 2H2O); DISSOLVE
it in water; TRANSFER all of it into a 500 ml volumetric flask;
DILUTE it to the mark; SHAKE to make it uniform.
2. WEIGH 0.718 g of barium carbonate which was dried at 110 ??C
to constant mass; ADD 1 + 4 hydrochloric acid solution to
dissolve it; TRANSFER all of it into a 500 ml volumetric flask;
DILUTE it to the mark; SHAKE to make it uniform.
Bismuth
(Bi)
1 mL solution
contains 1 mg of
bismuth (Bi)
1. WEIGH 1.616 g of bismuth nitrate [Bi (NO3)3 ?€? 5H2O]; ADD 50
ml of 1 +4 hydrochloric acid solution to dissolve it; TRANSFER all
of it into a 500 ml volumetric flask; DILUTE it to the mark; SHAKE
to make it uniform.
2. WEIGH 0.100 g of metal bismuth; DISSOLVE it in 6 mL of nitric
acid; BOIL it to remove nitrogen dioxide gas; TRANSFER all of it
into a 100 ml volumetric flask; DILUTE it to the mark; SHAKE to
Appendix A
(Informative)
Calibration of sulfur impurity standard solution
As for the sulfur (S) impurity standard solution which is prepared using the method 2 of Table 2 in clause 5.2, it may be calibrated using the following method if necessary.
ADD 10 mL of 1 mol/L zinc acetate solution into 250 mL iodine flask; PIPETTE 10.00 mL of sulfur [sulfide (by S)] and 20.00 mL of iodine standard solution [c (1/2I2) ???0.1 mol/L]; USE water to dilute it to 60 mL; ADD 5 mL of (1 + 5) sulfuric acid solution; tightly APPLY the water seal; SHAKE it uniformly; PLACE it in the dark for 5 min; USE the sodium thiosulfate standard titration solution [c (Na2S2O3) ???0.1 mol/L] to titrate the solution until it is in light yellow; ADD 1 mL of starch indicator solution; CONTINUE titration until the blue color disappears. Meanwhile USE 10 mL of water to substitute the sulfur impurity standard solution to make blank test.
The sulfur (S) content in the sulfur impurity standard solution is calculated by the mass concentration ?? of sulfur (S), it is expressed in (mg/mL), AND it is calculated in accordance with the formula (A.1).
Where.
V1 ?€? The volume value of the sodium thiosulfate standard titration solution as consumed to titrate the sulfur...

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