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INTERSTATE STANDARD

REAGENTS

AMMONIUM CHLORIDE

TECHNICAL CONDITIONS

Official edition

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of Chemical Industry of the USSR

2. APPROVED AND INTRODUCED BY Decree State Committee standards of the Council of Ministers of the USSR dated 27.04.72 No. 861

3. MS ISO 6353-2-83 (R. 5) has been introduced into the standard in terms of qualification x. h.

5. REFERENCE REGULATIONS AND TECHNICAL DOCUMENTS

6. The limitation of the validity period was removed according to protocol No. 5-94 of the Interstate Council for Standardization, Metrology and Certification (NUS 11-12-94)

7. EDITION (June 2007) with Amendments No. 1, 2, 3, approved in February 1980, July 1985, March 1990 (IUS 3-80, 10-85, 6-90)

Editor M. I. Maksimova Technical editor O. N. Vlasova Proofreader R. A. Mentova Computer proofing V. I. Grishchenko

Signed for publication on 22.06.2007. Format 60х84*/8 - Offset paper. Headset Times. Offset printing. Uel. oven l. 0.93.

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FSUE STANDARTINFORM, 123995 Moscow, Granatny per., 4. www.gostinfo.ru [email protected] Typed in FSUE "STANDARTINFORM" on a PC Printed in the branch of FSUE "STANDARTINFORM" - type. "Moscow printer", 105062 Moscow, Lyalin per., 6.

INTERSTATE STANDARD

Reagents AMMONIUM CHLORIDE Specifications

reagents. ammonium chloride. Specifications

MKS 71.040.30 OKP 26 2116 0920 01

Date of introduction 01.07.73

This standard applies to ammonium chloride.

Ammonium chloride is a white fine crystalline powder, soluble in water.

Formula: NH 4 C1.

Molecular weight (according to international atomic masses 1971) - 53.49.

1. TECHNICAL REQUIREMENTS

1.1a. Ammonium chloride must be manufactured in accordance with the requirements of this standard according to the technological regulations approved in the prescribed manner.

Official edition

1.1. In terms of physico-chemical parameters, ammonium chloride must comply with the standards specified in the table.

Reprint prohibited

© Standartinform, 2007

(Changed edition, Rev. No. 2, 3).

1a. SAFETY REQUIREMENTS

la. 1. Ammonium chloride can cause irritation of mucous membranes and skin.

The maximum permissible concentration in the air of the working area is 10 mg / m 3, the hazard class is 3 (moderately dangerous) according to GOST 12.1.007.

1a.2. When working with the drug, it is necessary to use individual means protection (respirators, goggles, rubber gloves), as well as observe the rules of personal hygiene.

(Introduced additionally, Rev. No. 1).

1a.3. Premises in which work with the drug is carried out must be equipped with supply and exhaust mechanical ventilation.

The analysis of the drug should be carried out in a laboratory fume hood. In places of the greatest dusting, local suctions are provided.

(Revised edition, Rev. No. 3).

2. ACCEPTANCE RULES

2.2. Mass fractions of nitrates, chlorates and other oxidizing agents, arsenic and heavy metals are determined by the manufacturer in every 20th batch.

(Introduced additionally, Rev. No. 3).

3. METHODS OF ANALYSIS

3.1a. General instructions for the analysis - according to GOST 27025.

Weighing using laboratory scales general purpose types VLR-200 g and VLKT-500g-M or VLE-200 g.

It is allowed to use other measuring instruments with metrological characteristics and equipment with technical specifications not worse, as well as reagents in quality not lower than those specified in this standard.

(Revised edition, Rev. No. 3).

pipettes 4(5)-2-1(2) and 6(7)-2-25;

cup for weighing SV-14/8 in accordance with GOST 25336;

distilled water, not containing carbon dioxide; prepared according to GOST 4517; sodium hydroxide according to GOST 4328, concentration solution c (NaOH) \u003d 0.1 mol / dm 3 (0.1 i.) and concentration solution c (NaOH) \u003d 0.5 mol / dm 3 (0.5 i.), prepared according to GOST 25794.1; rectified technical ethyl alcohol in accordance with GOST 18300 of the highest grade; phenolphthalein (indicator), alcohol solution with a mass fraction of 1%, prepared according to GOST 4919.1; formalin technical according to GOST 1625, solution 1:1, previously neutralized by phenolphthalein with a solution of sodium hydroxide at a concentration of 0.1 mol/dm 3 until a pink color that does not disappear within 20 s appears against the background of milk glass.

3.2.2. Conducting an analysis

About 0.8000 g of the drug is placed in a conical flask, dissolved in 40 cm 3 of water, 2-3 drops of phenolphthalein solution, 25 cm 3 of formalin solution (with a pipette) are added and titrated from a burette with a sodium hydroxide solution of a concentration of 0.5 mol / dm 3 to pink solution.

3.2.3. Results processing

The mass fraction of ammonium chloride (X) as a percentage is calculated by the formula

x \u003d Y-0.02674 100 t '

where V is the volume of a sodium hydroxide solution with a concentration of exactly 0.5 mol / dm 3 used for titration, cm 3; t is the weight of the sample of the preparation, g;

0.02674 - the mass of ammonium chloride corresponding to 1 cm 3 of sodium hydroxide solution with a concentration of exactly 0.5 mol / dm 3, g.

The result of the analysis is taken as the arithmetic mean of the results of two parallel determinations, the absolute discrepancy between which does not exceed the allowable discrepancy equal to 0.2%.

The permissible absolute total error of the analysis results is + 0.4% at a confidence level P = 0.95.

3.2.2; 3.2.3. (Changed edition, Rev. No. 2, 3).

3.3. Determination of the mass fraction of water-insoluble substances

3.3.1. Reagents and glassware:

3.3.2. Conducting an analysis

50.00 g of the drug is placed in a glass and dissolved by heating in 200 cm 3 of distilled water. The beaker is covered with a watch glass, heated for 1 hour in a water bath, and the solution is filtered through a filter crucible, previously dried to constant weight and weighed (the result of weighing in grams is recorded to the fourth decimal place). The filter residue is washed with 100 cm 3 of hot water and dried in an oven at 105-110°C to constant weight.

The preparation is considered to comply with the requirements of this standard if the mass of the dry residue does not exceed:

for the drug "chemically pure" - 1.0 mg; for the drug "pure for analysis" - 1.0 mg; for the drug "pure" - 5.0 mg.

Permissible relative total error of the analysis result for the drug "chemically

pure” and “pure for analysis” - +45%, for the drug “pure” - ±5% with a confidence level P = 0.95.

3.3.1; 3.3.2. (Revised edition, Rev. No. 3).

3.4. Determination of the mass fraction of the residue after calcination

The determination of the residue after calcination is carried out according to GOST 27184. In this case, 20.00 g of the drug is placed in a platinum crucible in parts and carefully heated on an electric stove until the bulk of the drug has volatilized.

The residue after calcination is retained to determine the mass fractions of calcium by and. 3.10 and magnesium according to and. 3.11.

(Changed edition, Rev. No. 1, 3).

3.5. Determination of the mass fraction of nitrates, chlorates and other oxidizing agents

At the same time, 5.00 g of the drug is placed in a conical flask with a capacity of 100 cm 3 (with a mark of 50 cm 3), dissolved in 25 cm 3 of water, 1 cm 3 of the solution is added of hydrochloric acid, heated to a boil and boiled for 1-2 minutes. The solution is cooled and then the determination is carried out by the sulfosalicylic method.

The preparation is considered to comply with the requirements of this standard if the mass of iron does not exceed:

0.010 mg - for the drug "chemically pure";

0.015 mg - for the drug "pure for analysis";

0.050 mg - for the drug "pure".

It is allowed to complete the definition visually.

In case of disagreement in the assessment mass fraction iron analysis is completed photometrically. (Revised edition, Rev. No. 2).

3.10. Determination of the mass fraction of calcium (Changed edition, Rev. No. 2).

3.10.1. Equipment, reagents and solutions: flask 2-200-2 according to GOST 1770; pipettes 6(7)-2-5 and 4(5)-2-1(2); test tube P4-15-14/23 XC according to GOST 25336; distilled water according to GOST 6709;

paper indicator universal.

3.10.2. Conducting an analysis

The residue after calcination, obtained according to paragraph 3.4, is dissolved by heating on a water bath in 1 cm 3 of a hydrochloric acid solution and 10 cm 3 of water. The solution is quantitatively transferred into a volumetric flask, the volume of the solution is adjusted to the mark with water and mixed - solution A; the solution is retained for the determination of magnesium according to clause 3.11.

5 cm 3 of solution A (corresponding to 0.5 g of the drug) is placed with a pipette in a test tube, neutralized with a solution of sodium hydroxide according to universal indicator paper (take-away sample), the volume of the solution is adjusted to 8 cm 3 with water, 1 cm 3 of sodium hydroxide solution is added, mixed , add 1 cm 3 solution of murexide and mix again.

The drug is considered to comply with the requirements of this standard if the pinkish-violet color of the analyzed solution in pink, observed after 1-2 minutes in transmitted light against the background of milk glass, is not more intense than the color of the reference solution prepared simultaneously with the analyzed one and containing in the same volume: for the drug "chemically pure" - 0.005 mg Ca; for the drug "pure for analysis" - 0.005 mg Ca; for the drug "pure" - 0.005 mg Ca;

1 cm 3 sodium hydroxide solution and 1 cm 3 murexide solution. The color of the solution is stable for 10 minutes.

3.10.1; 3.10.2. (Changed edition, Rev. No. 2, 3).

3.11. Determination of the mass fraction of magnesium

3.11.1. Equipment, reagents and solutions:

flask Kn-1-50-14/23 THS or Kn-2-50-18 THS according to GOST 25336; pipettes 4(5)-2-1(2) and 6(7)-2-5(10); distilled water according to GOST 6709;

Kind and type of container: 2-1, 2-4, 2-9, 6-1, 6-3, 11-1, 11-4.

Packing group: III, IV, V, VI, VII.

Danger signs are applied to the shipping container in accordance with GOST 19433 (class 8, subclass 8.1, drawing 8, classification code 8113) and the UN serial number 1759.

(Changed edition, Rev. No. 1, 2, 3).

4.2. (Deleted, Rev. No. 3).

4.3. The drug is transported by all means of transport in accordance with the rules for the carriage of goods in force on this type of transport.

4.4. The drug is stored in closed containers in covered warehouses.

5. MANUFACTURER WARRANTY

5.1. The manufacturer guarantees the compliance of ammonium chloride with the requirements of this standard, subject to the conditions of transportation and storage.

5.2. The guaranteed shelf life of the drug is three years from the date of manufacture.