tanzania bureau of standards€¦ · zeolite slurry first and then spray dried to form zeolite...

TBS/CDC 2 (5793) P3

© TBS 2019 All right reserved First Edition 2019

DRAFT TANZANIA STANDARD

TBS/CDC 2 (5793) P3 Zeolite - detergent grade- Specification

TANZANIA BUREAU OF STANDARDS

TBS/CDC-2(5795) P3

©TBS 2019 All right reserved First edition 2019

Foreword This Draft Tanzania Standard was developed by the Soap and Detergents Technical Committee under supervision of the Chemicals Divisional Standards Committee and it is in accordance with the procedures of the Bureau.

In the preparation of this Draft Tanzania Standard assistance was drawn from IS 15267:2003 (Reaffirmed 2013) Zeolite Detergent Grade - Specification; published by the Bureau of Indian Standards.

In reporting the results of analysis of a test if the final value is to be rounded off, it shall be done in accordance with TZS 4 Rounding off numerical values

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Introduction

Research and investigation found that Zeolite is the most suitable and ideal replacement for Sodium tripolyphosphate

(STPP) as the main builder in most of the detergents due to eutrophication effect to the water sources which is

caused by STTP affecting the life of living organisms especially aquatic organisms hence aquatic-ecosystem

disturbed.

Zeolite is synthesized normally in two different ways:

a) from amorphous hydrogels prepared from high purity sources of sodium silicates and sodium aluminates, and

b) from kaolin by calcinations followed by reaction with aqueous sodium hydroxide.

The formula of zeolite, normally used by detergent industry is Na12(AlO2.SiO2)12.27H2O. Zeolite is manufactured as

zeolite slurry first and then spray dried to form zeolite powder. In the spray dried detergent manufacturing process,

zeolite is used in the slurry form and spray drying in the zeolite plant is hence eliminated. Zeolite whenever dispatched

in the slurry form is stabilized and sent under the nomenclature ‘Zeolite master batch.

Zeolite in powder form is used in detergent cakes and in detergent powders prepared by dry mixing process is

generally used as a builder in detergent industry. Since it causes eutrophication, there was intensive research for an

alternative to STPP. After rigorous

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TBS/CDC-2(5793) P3

Zeolite Detergent Grade - Specification

1 Scope

This Draft Tanzania Standard specifies requirements, sampling and test methods for Zeolite - detergent grade.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.

TZS 59/ISO3696 Water for analytical laboratory use – Specification and test method

TZS 219 Sodium silicate - Specification

3 Terms and definitions

Not applicable

4 Requirements

4.1 General requirements

Zeolite powder shall be in the form of fine powder, white in colour. It essentially consists of hydrated sodium alumino- silicates. It is odourless and non-hygroscopic inorganic material.

4.2 Specific requirements

The material shall also comply with the specific quality requirements given in Table 1, when tested in accordance with the method prescribed therein.

DRAFT TANZANIA STANDARD

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Table 1 — Specific requirements for Zeolite detergent grade

S/No Characteristic Requirement Method of test

i) Average particle size as μm, max 5.0 Annex A

ii) Sieve-residue (50 microns sieve), percent by mass,

max

0.5 Annex B

iii) Bulk density, g/L, min 500 Annex C

iv) Relative brightness, min 94 Annex D

v) pH of 5% suspension 10.7-11.7

vi) Assay content, percent by mass 77.5-79.5 Annex E

vii) Calcium binding capacity (as mg CaO/g assay), min 155 Annex F

viii) Average chemical composition:

• Sodium (as Na2O), percent by mass

• Aluminium (as AI2O3), percent by mass

• Silica (as SiO2, percent by mass

16.5 -17.5

27.5 -28.5

32.5 -33.5

Annex G

5 Packaging and labelling

5.1 Packaging

The material shall be packaged in dry containers that are strong enough to withstand normal handling and transportation and that will prevent contamination of the product.

5.2 Labelling

The container shall be securely closed, legibly and indelibly marked with the following information:

a) name of the product as “Zeolite – detergent grade”

b) manufacturer’s name and physical address;

c) recognized trade mark (if any).

d) batch or lot number;

e) net content;

f) country of origin;

g) date of manufacture.

h) Expiry date

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6 Sampling

Representative samples of the material shall be drawn and their conformity to this standard shall be determined in

accordance with the method prescribed in Annex H.

7 Quality of reagents

Unless specified otherwise, analytical grade chemicals and Water for analytical laboratory (see TZS 59/ISO 3696)

shall be used in tests.

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Annex A (normative)

Determination of average particle size

A.1 Apparatus A.1.1 Coulter Counter — 100μ and 50μ aperture tube.

A.1.2 Ultrasonic Cleaner

A.1.3 Beakers— 100 mL capacity

A.1.4 Micro Pipettes

NOTE-— All apparatus should be scrupulously clean and dust free

A.2 Reagent Sodium Chloride Solution - 0.5% which shall be filtered through 0.2μ filter. A.3 Procedure A.3.1 Calibration of the Instruments 0.1 of the standard 10μ latex suspended in 50 mL sodium chloride solution and placed in an ultrasonic cleaner for 2 min. put a magnetic pellet and stir for 2 min in magnetic stirrer. By using variable pipette, transfer exactly400μL of suspension into 150mL of sodium chloride solution in a cup of the Coulter-counter. Preliminary arrangements shall be done asper instrument manuals. Calibrate the system. A.3.2 Test Procedure 0.1 g of the zeolite powder is suspended in 50 mL sodium chloride solution and placed in an ultrasonic cleaner for 2 min. Put a magnetic pellet and stir for 2 min in magnetic stirrer. By using variable pipette, transfer exactly 400 μL of suspension into 150mL of sodium chloride solution in a cup of the Coulter counter. Preliminary arrangements shall be done asper instrument manuals. The suspension should be scanned for 60 μ to 1.0 μ. The number of particles present in each interval of particle size range is found and hence the average size calculated.

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Annex B

(normative)

Determination of sieve-residue

B.1 General

The Mocker method is used to determine big and firm agglomerates of zeolite crystals which may remain onthe

textile after washing using zeolite containing detergents.

B.2 Apparatus

B.2.1 Mocker Apparatus

B.2.2 Sieve - 50 microns

B.2.3 Air drying oven

B.2.4 Water Jet Vacuum Pump

B.2.5 Beaker- 400 mL capacity

B.2.6 Stirrer

B.3 Procedure

5 g of the sample is weighed into a beaker, mixed with100 mL of hot distilled water and suspended with a glass

stirrer. A 50μ sieve is attached to the Mocker apparatus. The Mocker apparatus is made ready as per instructions

given by the supplier. Then the suspension is poured into the Mocker apparatus by means of a funnel and sieved at

a -water pressure of (0.3 -0.5) kg/cm2 (150 L/h). The suspension is added in portions, so that the filtering surface

keeps as free as possible. When the major quantity of the sample has passed through the sieve, the noise of the

water jet changes. It becomes louder and hissing noise is heard. Continue to sieve for 3 min more. Then the

apparatus is switched off, the test sieve is removed and dried in the oven at110°C for 30 min. The sieve is cooled

and weighed to constant mass. Then the residue is carefully removed and the empty sieve is weighed again.

B.4 Calculation

Sieve-residue, percent = 𝑀 ×100

𝑀1

where

M = amount of dried residue, in g (difference in mass of sieve), and

𝑴𝟏= mass of powder taken in g.

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Annex C

(Normative)

Determination of Bulk density of Zeolite powder

C.1 General The volume of specified mass of powder after 250 taps is determined and hence the bulk density is found. C.2 Apparatus

C.2.1Bulk density apparatus C.2.2Graduated cylinder - 50 mL capacity. C.2.3Funnel - wide and short stemmed C.3 Procedure

Rest the funnel over the top edge of the tared graduated cylinder. Fill the cylinder to the 50 mL mark by pouring the material through the funnel, without tapping and level the powder with the minimum of disturbance. Leave the cylinder untouched for 5 min and add more powder, if necessary, to bring the contents to the 50 mL mark, level again with the minimum of disturbance weigh the filled cylinder stopper the tilled cylinder and tit it in the bulk density apparatus and give 250 taps by motor arrangement of the apparatus. Note the volume of the material after compacting. C.4 Calculation

Bulk density = 𝑀 ×1 000

𝑉

where

M=mass of powder, in g, and

V = volume, in ml, of powder after 250 taps.

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Annex D

(normative)

Determination of relative brightness

D.1 General

The relative brightness of the zeolite powder is determined by reflectance meter.

D.2 Apparatus

Gloss reflectance meter.

D.3Procedure

The zero adjustment of the reflectance meter is first done by placing the reflectance head on a black plate. Then the

hundred adjustment is done by placing the reflectance head on a perfectly white magnesia block or barium sulphate

crystals packed in a suitable cup. The zeolite powder is packed in a similar cup such that the top layer is perfectly

plain and the reflectance is measured as in the above manner. The instrument reading corresponds to the percentage

of relative brightness.

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Annex E

(normative)

Determination of assay

E.1 Apparatus

E.1.1Platinum crucible - 20 mL. E.1.2Drying oven E.1.3Muffle furnace E.1.4Desiccator E.2 Procedure

2.5 g of the powder sample is weighed to exactly 0.1 mg into a 20 mL platinum crucible, which has been heated at

800⁰C and cooled in desiccators. Then the sample is heated in a muffle furnace for 1 h at800⁰C. After cooling in the

desiccator, weigh the crucible to constant mass. E.3 Calculation

Zeolite, percent by mass =(𝑀1−𝑀2) ×100

𝑀3

where

𝑀1= mass of platinum crucible and sample after heating, in g;

𝑀2 = mass of platinum crucible, in g; and

𝑀3 = mass of sample, in g

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Annex F

(normative)

Determination of the Calcium-binding-capacity (CaBC)

F.1 Apparatus

F.1.1 Measuring flask - 100 mL

F.1.2 Pipette - 200 mL

F.1.3 Beaker - 400 mL

F.1.4 Erlenmeyer flask - 300 mL

F.1.5 Magnetic stirrer

F.1.6 Filter paper Whatman No. 42

F.2 Reagents

F.2.1 Calcium chloride- reagent grade

F.2.2 Sodium hydroxide solution - 0.5 N

F.2.3 Patten Reeder’s Indicator - 1% (m/v).Mix 1.0 g of solid indicator [2 hydroxy -1-(2 hydroxy-4- sulpho - 1 -

napthylazo) -3- naphthoic acid -(HHSNNA)] with 99 g of pure sodium chloride or sodium sulphate anhydrous in a

mortar and pestle and grind well to about 250 to 150 μ, mixing it intimately so as to make the diluted reagent powder

homogeneous. Preserve in a tightly stoppered amber-coloured bottle.

F.2.4 EDTA Solution - 0.1 M

F.2.5 Calcium Chloride Solution - Dissolve 0.5937g of calcium chloride or0.786 5 g of CaCl2. 2H20 in distilled water.

Adjust the pH to 10 by addition of 2 N sodium hydroxide solution. Transfer 100 mL of this solution into an Erlenmeyer

flask. Add Patten Reeder’s indicator and 10 ml of 0.5 N sodium hydroxide solution. Titrate with0.1 M EDTA solution

till the colour changes from pink to blue. This solution will contain300 ppm of calcium.

F.3 Procedure

Take 200 mg of zeolite powder, exactly weighed to 0.1 mg in a beaker. Add200 mL of the standardizedCaCl2 solution,

at 25°Cexactly, with continuous stirring with a magnetic stirrer for 10 min. Filter immediately through Whatman No.

42 filter paper. Take 100 ml of the filtrate into an Erlenmeyer flask. Add Patten Reeder’s indicator and10 mL 0.5 N

sodium hydroxide and titrate with 0.1 NEDTA solution till colour changes from pink to blue. Also, carry out a blank

without the zeolite sample.

NOTE —The temperature shall be maintained at 25°C throughout the experiment.

F.4 Calculation

CaBC (mg CaO/g assay) =(𝑉1−𝑉2) ×𝑀 ×28 ×2

𝑚 ×𝑎𝑠𝑠𝑎𝑦 𝑐𝑜𝑛𝑡𝑒𝑛𝑡

where

𝑉1 = volume of EDTA consumed for blank,

𝑉2= volume of EDTA consumed with the sample,

𝑀 = Molarity of EDTA, and

𝑚 = mass of zeolite sample

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Annex G

(normative)

Determination of Average chemical composition of Zeolite powder

G.1 General The chemical composition of zeolite is determined volumetrically. G.2 Determination of Aluminium (as Al2O3)

G.2.1 Reagents

G.2.1.1 Disodium Ethylenediamine Tetra Acetate (EDTA) Solution - 0.05M.

Dissolve 18.6125 g of disodium ethylenediamine tetra acetate dihydrate in water and make the volume to one litre in a volumetric flask.

G.2.1.2 Concentrated Sulphuric Acid

G.2.1.3 Hexamine (Hexamethylene Tetramine) Analar

G.2.1.4 Xylenol Orange Indicator

Prepare 0.5 percent in water and add 1 to 2 drops of dilute sodium hydroxide solution.

G.2.1.5 Standard Lead Nitrate Solution - 0.05 M.

G.2.2 Procedure

Dissolve 5 g of prepared sample in water. Acidify it by adding 1 to 2 ml of concentrated sulphuric acid and make up the volume to 500 ml in a volumetric flask. Take an aliquot of 50 011 into a conical flask. Add 50 ml of 0.05 M EDTA solution and heat to just boiling. Cool it and add hexamine powder to adjust the pH to 5. Add few drops of xylenol orange indicator. Titrate the excess EDTA solution with standard lead nitrate solution until the colour changes from yellow to pink.

G.2.3 Calculation

Calculate the aluminium content of the material on the assumption that one milliliter of 0.05 M EDTA solution is equivalent to 0.002 55 g of aluminium (as Al2O3).

G.3 Determination of Silica (as SiO2,)

Weigh 10 g of sample, dissolve in 1 M HCI and make up to 500 mL Dilute to the mark and mix well. Estimation of SiO2, is done as per G.5 G.4 Determination of Sodium (as Na2O)

Sodium percent by mass is calculated as follows: Percent by mass (as Na2O) =Percent by mass assay – Percent by massAl2O3 –Percent by mass SiO2, G.5 Determination of total soluble silica (as SiO2) G.5.1 Reagents G.5.1.1 Concentrated hydrochloric acid G.5.1.2 Dilute hydrochloric acid – 1:1 by volume. G.5.1.3 Concentrated sulfuric acid

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G.5.1.4 Hydrofluoric acid – About 40 percent (w/v) G.5.2 Procedure Take 50 ml of the prepared sample solution (see G.3) in a 150 ml porcelain evaporating dish, add 25 ml concentrated hydrochloric acid and evaporate to dryness on a water-bath. Moisten the residue with 10 ml dilute hydrochloric acid and again evaporate to dryness on a water-bath. Heat the dish for one hour on a hot plate maintained at 110 ºC ± 5 ºC. To dissolve the soluble salts, add 10 ml of dilute hydrochloric acid and 20 ml of water to the residue and digest for 5 minutes on the water-bath. Filter the residue, which is mainly silica, through a Whatman filter paper and wash the residue on the filter paper with hot water till it is free from chlorides. Keep the residue on the filter paper and collect the filtrate and washings in original dish. G.5.2.1 Evaporate to dryness the filtrate and washings on the water-bath; moisten the residue with 10 mL dilute hydrochloric acid and again evaporate to dryness. Heat at 110 ºC ± 5 ºC for one hour, add to the residue 10 ml of dilute hydrochloric acid and 20 ml of water and digest as before to dissolve the soluble salts. Filter any additional silica separated on a separate filter paper and wash it free from chlorides as before. G.5.2.2 Transfer both the filter papers and the residues as obtained under A.5.2 and A.5.2.1 to a platinum crucible previously ignited and weighed without cover. Ignite it in a muffle furnace, slowly raising its temperature until free from carbon. Cover the crucible with a platinum cover, heat to the highest temperature of blast burner for 15 minutes. Cool in a desiccator and weigh without the crucible cover. G.5.2.3 Add sufficient water just to moisten the contents of the crucible and add 2 to 3 drops of concentrated sulfuric acid. Slowly add 10 ml of hydrofluoric acid. Evaporate to a small volume on the water-bath; add another portion of about 10 ml of hydrofluoric acid and evaporate to fumes of sulfuric acid. Heat the crucible gently at first over an open flame to drive off sulfuric acid and finally at a red heat. Cool in a desiccator and weigh. Repeat the heating, if necessary, till constant weight is obtained. G.5.3 Calculation Total soluble silica (as SiO2), Percentage by weight = 1 000 x A - B W Where A is the weight in g of the residue and crucible as obtained under G.5.2.2, B is the weight in g of the residue and crucible after treatment with hydrofluoric

acid (see G.5.2.3), and W is the weight in g of the material of taken for the prepared sample solution

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Annex H

(normative)

Sampling of Zeolite powder

H.1 General Requirements

H.1.1 In drawing, preparing, storing and handling samples, the following precautions shall be observed.

H.1.1.1 Samples shall be taken in a protected place, not exposed to damp air, dust or soot.

H.1.1.2 The sampling instruments shall be clean and dry when used.

H.1.1.3 The samples, the material being sampled, the sampling instruments and the containers for samples shall be

protected from adventitious contamination.

H.1.1.4 The samples shall be placed in clean and dry glass containers. The sample containers shall be of such a

size that they are almost completely filled by the sample.

H.1.1.5 Each container shall be sealed airtight after filling and marked with full details of sampling, date of sampling,

batch or code number, name of manufacturer, and other important particulars of the consignment.

H.1.1.6 The samples shall be stored in such a manner that the temperature of the material does not vary unduly from

the normal state and that they are protected from light.

H.2 Scale of Sampling

Lot

H.2.1 In a single consignment, all the packages containing material of the same type, and drawn from the same

batch of manufacture, shall constitute a lot.

H.2.2 For ascertaining the conformity of the lot to the requirements prescribed in this standard, tests shall be carried

out on each lot separately. The number (n) of bags to be selected for drawing the sample shall depend upon the size

(N) of the lot, and shall be in accordance with Table 2.

Table 2 Scale of Sampling

SL. N Lot size Sample size

1. Up to 50 3

2. 51 to 100 4

3. 101to300 5

4. 301 to 500 7

5. 50 I and above 10

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H.2.3 The bags shall be selected at random. In order to ensure the randomness of selection, a random number table

shall be used. In the absence of a random number table, the following procedure may be adopted: Starting from any

package in the lot, count them in one order as 1, 2, 3, up to r and so on where r is the integral part of N/n (N being

the lot size and n the number of bags to be selected). Every rth package thus counted shall be withdrawn to give the

required sample size’.

H.3 Preparation of gross samples,

Test samples and reference samples

H.3.1 Gross Samples

H.3.1.1 From each one of the bags selected as in H.2, draw at random one or more containers. The material in the

containers so chosen shall be nearly thrice the quantity required for purposes of test as indicated in H.4.

H.3.1.2 The material from the containers-selected as in H.3.1.1 shall be disintegrated, if necessary, and mixed

thoroughly to give the gross sample for the bag.

H.3.2 Test Samples

H.3.2.1 Segregate carefully the gross samples. From each gross sample, take a small but equal quantity of material

and mix it thoroughly into a composite sample which should be of a size sufficient to carry out triplicate test for all

the characteristics specified under H.4. The composite sample shall be divided into three equal parts, one for the

purchaser, and another for the supplier, and the third for the referee.

H.3.2.2 The remaining portion of the material in each one of the gross samples shall be divided into three equal

parts, each forming an individual sample. One set of individual samples representing the n selected bags for the

purchaser, another for the supplier, and the third for the referee.

H.3.2.3 All the composite and individual samples shall be transferred to separate containers. These containers shall

then be sealed airtight with stoppers, and labeled with full particulars of identification given in H.1.1.5.

H.3.3 Reference samples

H.3.3.1 The reference samples shall consist of a composite sample and a set of n individual samples. All the

containers shall bear the seals of both the purchaser and the supplier, and shall be kept at a place agreed to between

the two parties.

H.3.3.2 Reference samples shall be used in cases of any dispute between the purchaser and the supplier.

H.4 Number of Tests

H.4.1 Tests for the determination of active ingredient shall be performed on each of the individual samples.

H.4.2 Tests for the determination of the remaining characteristics given in Table 1 shall be conducted on the

composite sample.

H.5 criteria for conformity

H.5.1 For Individual Samples

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For the characteristic which has been determined on the individual sample, the mean (x̅) and the range (R)of test

results shall be calculated as follows:

Mean (x̅) =Sum of test results

Number of test results

Range (R) = Difference between the maximum and minimum values of test results.

NOTES

1. The value of the expression (x̅— kR) shall be calculated from the relevant test results [see also Note 2]. If the value so

obtained is greater than or equal to the minimum limit, the lot shall be declared as conforming to the requirement for that

characteristic.

2. The value of the factor k referred to in Note 1 shall be chosen in accordance with Table 3, depending upon the acceptable

quality level, that is, the percentage of nonconforming bags that may be tolerated reasonably.

Table 3 Value of ‘k’ for Achieving Different

SL. N Acceptable Quality Level Value of ‘k’

1. Not more than 3.0 percent defective 0.4

2. Not more than 1.5 percent defective 0.5

3. Not more than 0.5 percent defective -

H.5.2 For Composite Sample

For declaring the conformity of the lot to the requirements of all the remaining characteristics determined on the

composite sample, the test results for each one of the characteristics satisfies the relevant requirement given in

Table 1.

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tanzania bureau of standards€¦ · zeolite slurry first and then spray dried to form zeolite...

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