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    FOR COMMENT ONLY

    PROPOSAL FOR A

    TRINIDAD AND TOBAGO STANDARD

    COMPULSORY

    DETERGENT SYNTHETIC LAUNDRY DETERGENT POWDER SPECIFICATION

    PCTTS 466: 20XX(1st Revision)

    Date of Issue: Closing Date for Comments:2009-06-08 2009-08-06

    Send Comments to:

    The Executive Director,

    TRINIDAD AND TOBAGO BUREAU OF STANDARDSCentury Drive, Trincity Industrial Estate,

    Macoya, TUNAPUNAP.O. Box 467, PORT OF SPAIN,

    Trinidad and TobagoTelephone: 662-8827, 662-3810, 663-4835/6

    Telefax: 663-4335; E-mail: [email protected]

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    General Statement

    The Trinidad and Tobago Bureau of Standards (the Bureau) is a body corporate established under

    the authority of the Standards Act No. 18 of 1997 (herein after referred to as the Standards Act).

    In accordance with the Standards Act, the Bureau shall promote and encourage the development and

    maintenance of standards and further shall establish standards for the following: to improve goods

    produced or used in Trinidad and Tobago; to ensure industrial efficiency and development; to promote

    public and industrial welfare, health and safety; and to protect the environment.

    The Bureau develops standards through consultation with relevant interest groups, and public

    comment is invited on all draft standards before they are declared as Trinidad and Tobago Standards

    in accordance with the provisions of the Standards Act.

    The Bureau is the legal custodian of Trinidad and Tobago Standard Marks, which are issued in

    accordance with the Standards Act. When a Trinidad and Tobago Standard Mark appears on any

    product, or in connection with any service, process or practice, it provides assurance that such aproduct, service, process or practice conforms to a Trinidad and Tobago Standard.

    The Bureaus Standards Information Centre maintains a reference library of standards, including

    local, regional and international standards and is the national node of the International Organization

    for Standardization Information Network (ISONET). The Centre also acts as the sales agent for the

    publications of foreign and international standards organizations.

    NOTE In order to keep abreast of progress in the industries concerned, Trinidad and Tobago Standards are

    subject to periodic review. Suggestions for improvements are welcome.

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    AMENDMENTS ISSUED SINCE LAST PUBLICATION

    AMENDMENT NO. DATE OF ISSUE TEXT AFFECTED

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    ATTACHMENT PAGE FOR TTBS AMENDMENT SHEET

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    TRINIDAD AND TOBAGO STANDARD

    DETERGENT SYNTHETIC LAUNDRY DETERGENT POWDER SPECIFICATION

    (1st

    Revision)___________________________________________________________________________________

    The Committee responsible for the development of this Trinidad and Tobago Standard is as follows:

    Specification Committee for synthetic laundry detergent powder

    Members Representing

    Ms Denrica Christopher (Chairperson) Ministry of Legal Affairs, Consumer AffairsDivision

    Mr Douglas Clarke Hi Lo Food Stores

    Ms Vidia Persad Doodnath Trinidad and Tobago Manufacturers' Association

    Mr Damian George Genethics Pharmaceuticals Limited

    Mr Vivian George Ministry of Health, Chemistry, Food and DrugsDivision

    Mr Alexei Nimblett Caribbean Industrial Research Institute

    Mr Ramon O'Brien Unilever Caribbean Limited

    Mr Ryan Sooklalsingh Alstons Marketing Company Limited

    Ms Karlene Lewis Trinidad and Tobago Bureau of Standards,Laboratory Services Division

    Ms Reesa Thomas Trinidad and Tobago Bureau of Standards,Implementation Division

    Mr Sheva Serrattan (Technical Secretary) Trinidad and Tobago Bureau of Standards,Standardization Division

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    Contents

    Foreword...........................................................................................................................................................1

    Introduction .......................................................................................................................................................2

    1 Scope ................................................................................................................................................... 3

    2 Normative references ...........................................................................................................................3

    3 Terms and definitions ...........................................................................................................................4

    4 Requirements ....................................................................................................................................... 64.1 General requirements...........................................................................................................................64.2 Specific requirements ...........................................................................................................................7

    5 Test methods........................................................................................................................................9

    6 Sampling ..............................................................................................................................................96.1 Sample size..........................................................................................................................................96.2 Selection of primary packages.............................................................................................................. 96.3 Selection of secondary packages ....................................................................................................... 10

    7 Conformity requirements ....................................................................................................................107.1 Lot conformity.....................................................................................................................................107.2 Conformity assessment ......................................................................................................................10

    8 Packaging and labelling...................................................................................................................... 11

    Annex A (normative) Determination of moisture and volatile matter content................................................... 12

    Annex B (normative) Determination of pH value............................................................................................. 13

    Annex C (normative) Determination of matter insoluble in water .................................................................... 14

    Annex D (normative) Determination of free alkali as NaOH............................................................................ 16

    Annex E (normative) Determination of net weight of product.......................................................................... 17

    Annex F (informative) Additional commonly used detergent ingredients ......................................................... 18

    Tables

    Table 1 Chemical and physical requirements .............................................................................................. 8

    Table 2 Scale of sampling............................................................................................................................ 9

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    Foreword

    This specification was declared a Trinidad and Tobago Standard on .., after the draft had

    been approved by the Trinidad and Tobago Bureau of Standards. This standard is a revision of TTS466: 2002 Detergent Synthetic laundry detergent powder Specification.

    This standard was revised to reflect the new format of Trinidad and Tobago standards and to keepabreast with current practices in the industry. This first revision differs from the original standard asfollows:

    a) performance requirements have been removed; and

    b) labelling requirements have been modified.

    The Trinidad and Tobago Bureau of Standards has recommended that this standard be declared acompulsory standard to protect the consumer or user against danger to health or safety.

    This revision will become effective as a compulsory standard on a date to be notified by the Ministerresponsible for trade and industrial development in a Notice to be published in the Trinidad andTobago Gazette, as required by the Standards Act.

    This national standard was developed for compliance by manufacturers, importers and distributors ofsynthetic laundry detergent powder.

    In formulating this standard considerable assistance was derived from the following publication whichwas still current when this standard was being developed:

    Bureau of Indian Standards

    IS 4955: 2001 Household laundry detergent powders Specification (Fourth revision)

    Annexes A, B, C, D, and E form a normative part of this standard. Annex F forms an informative partof this standard.

    Annex A outlines the procedure to determine moisture and volatile matter content.

    Annex B outlines the procedure to determine pH value.

    Annex C outlines the procedure to determine matter insoluble in water.

    Annex D outlines the procedure to determine the free alkali as sodium hydroxide.

    Annex E outlines the procedure to determine net weight.

    Annex F lists commonly used detergent ingredients.

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    Introduction

    Synthetic laundry detergent powder is a commonly used product in Trinidad and Tobago. It is

    customarily used for laundering by manual means or using automatic washing machines. Automaticwashing machines include traditional agitator washers in which the textiles or fabrics are completelysubmerged in water while an agitator moves the laundry back and forth to dislodge soils. In mostcases, traditional agitator washers are top-loading. Synthetic laundry detergent powder is typicallyformulated to be used in agitator washers. A considerable amount of water is required for thedetergent to perform the functions of removing and preventing the redeposition of soils.

    Due to increased environmental awareness, there is a need for more efficient detergents with adecreased environmental impact. Recent technological advances have led to the development ofmore efficient and environmentally friendly washers known as high efficiency washing machines.These washers are designed on the principle of a moving drum which creates a gentle tumblingmotion of the laundry to dislodge the soils. High efficiency washers can be either front-loading or top-loading and all front-loading washers are high efficiency.

    High efficiency detergents have been designed for use in these high efficiency washing machines.High efficiency washing machines utilize less water in their wash and rinse cycles and are relativelymore energy efficient. High efficiency detergents are formulated to be compatible with high efficiencywashing machines by producing reduced suds and by being more water-soluble. High efficiencydetergents are typically available in the liquid form and are not covered by this standard.

    This standard is intended to specify requirements for laundry detergent powder that is generally usedin traditional agitator washing machines. Laundry detergent powder is not easily dissolved in highefficiency washing machines because such detergents require more water than the volume that isused in high efficiency washing machines. Traditional detergents also require higher volumes of waterto prevent redeposition of soils, and excess suds production associated with these detergents candeter the mechanical operation of high efficiency washing machines. Ultimately, powdered laundrydetergent is typically not formulated for use in high efficiency washing machines.

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    1 Scope

    This national standard provides the specification for synthetic laundry detergent powder, herein

    referred to as detergent. It specifies the chemical and physical requirements identifying maximum andminimum permissible limits of key parameters. It also covers essential ingredients, test methods andrequirements for packaging, labelling and sampling.

    This national standard is applicable to synthetic laundry detergent powder intended primarily forwashing household textile products using conventional washing machines, or by manual means.

    This national standard does not apply to liquid laundry detergent.

    This national standard does not include methods for measuring the performance of synthetic laundrydetergent powder.

    2 Normative references

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

    ASTM International

    ASTM D 502-89 (Reapproved 2003), Standard test method for particle size of soaps and otherdetergents

    ASTM D 2667-89 (Reapproved 2008), Standard test method for biodegradability of alkylbenzenesulphonates

    British Standards Institution

    BS 1647: Part 1: 1984,pH Measurement Part 1. Specification for pH scale

    BS 1647: Part 2: 1984,pH Measurement Part 2. Specification for reference value standard solutionsand operational reference standard solutions

    BS 3145: 1978, Specification for laboratory pH meters

    BS 3762: Section 3.15: 1985, Analysis of formulated detergents Part 3. Quantitative test methods Section 3.15 Method for estimation of carboxymethylcellulose content

    BS 3762: Section 3.7: 1986,Analysis of formulated detergents Part 3. Quantitative test methods Section 3.7 Method for determination of total non-ionic matter content

    International Organization for Standardization

    ISO 2271: 1989, Surface active agents Detergents Determination of anionic-active matter bymanual or mechanical direct two-phase titration procedure

    ISO 2871-1: 1988, Surface active agents Detergents Determination of cationic-active mattercontent Part 1 High-molecular-mass cationic-active matter

    ISO 2871-2: 1990, Surface active agents Detergents Determination of cationic-active mattercontent Part 2: Cationic-active matter of low molecular mass (between 200 and 500)

    ISO 4313: 1976, Washing powders Determination of total phosphorous(V) oxide content - Quinolinephosphomolybdate gravimetric method

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    ISO 8215: 1985, Surface active agents Washing powders Determination of total silica Gravimetric method

    Trinidad and Tobago Bureau of Standards

    TTS 76: Part 15, Requirements for labelling Labelling of general household and automotive cleaningchemicals

    3 Terms and definitions

    For the purposes of this national standard the following terms and definitions shall apply.

    3.1

    active ingredientsthe organic surface active material present in the detergent

    NOTE Permissible types of active ingredient include anionic, cationic and non-ionic.

    3.2addressthe full postal address of the principal place of business or registered office of the manufacturer ordistributor of the cleaning chemical

    3.3agglomerationa mass of powder particles bound loosely together into a cluster

    3.4

    anionic surface active agent

    a surface active agent which ionizes in aqueous solution to produce negatively charged organic ionswhich are responsible for the surface activity

    3.5

    anti-redeposition agenta substance that inhibits the redeposition of suspended soil in a washing bath, that was previouslyremoved from the fabric

    3.6

    appropriate authoritya person, officer or authority administering a law regulating the importation, manufacture or use oftoxic chemicals

    3.7

    batchdetergent of a single type, grade, class and composition manufactured under the same conditions

    3.8

    biodegradablecapable of being decomposed into innocuous products by living matter

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    3.9

    buildera material added to the detergent formulation that enhances or maintains the cleaning efficiency of the

    surface active agent, principally by inactivating water hardness either by sequestration, precipitationor ion exchange

    NOTE Secondary benefits may include supplying alkalinity, buffering to maintain alkalinity at optimumeffective cleaning levels, adding anti-redeposition properties and emulsifying oily soil.

    3.10

    cationic surface active agent

    a surface active agent which ionizes in aqueous solution to produce positively charged organic ions

    which are responsible for the surface activity

    3.11

    defectanon-conformance with a requirement of the standard

    3.12

    defectiveunacceptable or unsuitable for distribution or sale as determined by conformity with this nationalstandard

    3.13

    detergenta composition that removes soil

    3.14

    distributorthe person or organisation actually engaged in the marketing of synthetic laundry detergent powder

    NOTE The manufacturer may be its own distributor.

    3.15

    foreign mattermatter not intended to be part of the detergent composition by the manufacturer

    3.16

    homogenoushaving a uniform structure and composition

    3.17

    laundry detergent powdera substance primarily intended for the wet-cleaning of household textile products, which contains asurfactant as an essential component for laundering fabrics

    3.18

    lotall the packages in a consignment containing material of the same grade and drawn from the samebatch

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    3.19

    manufacturerthe person or organization actually engaged in or principally responsible for manufacturing or

    producing the laundry detergent

    3.20

    mixed active ingredient detergenta detergent containing a mixture of surface active agents

    3.21

    moisture and volatile matterwater and other materials in a detergent that are volatile under the conditions of the test

    NOTE This test is detailed in Annex A.

    3.22

    non-ionic surface active agenta surface active agent which does not produce ions in an aqueous solution, but has functional groupswhich are responsible for its surface activity

    3.23

    primary packagethe unit in which the detergent is stored, which is labelled, and distributed for individual sale

    EXAMPLE It may be a carton, sachet, box or bag.

    3.24

    secondary packagea parcel consisting of primary packages of detergents, grouped together for ease of handling,transport, distribution or sale

    3.25

    soilmatter out of place, on the fabric, that is to be removed by the detergent

    3.26

    surface active agentsurfactanta material which when added to a liquid medium, modifies the properties of the medium at a surfaceor interface

    4 Requirements

    4.1 General requirements

    4.1.1 Physical appearance

    4.1.1.1 The detergent shall be homogenous in appearance and shall consist of non-segregating,free-flowing powder.

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    4.1.1.2 In the instance that caking or lumping occurs during normal storage, agglomerations mustbe capable of easy dispersal with little manual effort.

    4.1.1.3 The detergent shall be visibly free from foreign matter.

    4.1.2 Dispersibility

    The detergent shall be readily dispersible in water.

    4.1.3 Effect on health

    The manufacturer, importer and distributor of the finished product shall be able to provide evidencethat the product, when used in accordance with the stipulated directions, shall not cause any harm orthreat to human health or the environment.

    NOTE When washing by manual means, suitable protective measures should be taken against thedetergents typically drying nature. Further, persons bearing special topical sensitivity to detergents should alsotake the necessary precautions.

    4.1.4 Contents

    The net weight of the contents of the package shall not be less than that stated on the label asdetermined in accordance with Annex E.

    4.2 Specific requirements

    4.2.1 Storage properties

    The detergent shall meet the requirements stated in clauses 4.1.1 to 4.1.4, for a period of at leasttwelve (12) months from the date of manufacture, when stored according to the manufacturersinstructions.

    4.2.2 Ingredients

    4.2.2.1 The detergent shall contain the following as essential components:

    a) surface active agents;

    b) builders; and

    c) anti-redeposition agents.

    4.2.2.2 The detergent shall meet the requirements for biodegradability as specified in Table 1.

    NOTE The detergent may also contain special purpose additives to enhance performance, convenience, orproduct appeal. A list of commonly used ingredients is presented in Annex F.

    4.2.2.3 The detergent shall not contain any ingredient which poses a threat to human health orthe environment or is deemed unsuitable for use by the appropriate authority.

    NOTE For ingredients not known as suitable surfactants, builders or additives for laundry detergents, themanufacturer or distributor should provide evidence that such substances have been found to be harmless tohuman health and the environment and suitable for use as such.

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    4.2.3 Chemical and physical requirements

    The detergents properties shall comply with the requirements presented in Table 1 when analysed

    according to test methods specified for each property.

    Table 1 Chemical and physical requirements

    Property Limit Test Method

    Minimum Maximum

    Moisture and volatile mattercontent at 105 C max. (wt %)

    - 15 Annex A

    pH of 1 % aqueous solution at27 C

    9.0 11.0 Annex B

    Water insoluble matter (wt %) - 5.0 Annex C

    Free alkali as NaOH (wt %) - 0.1 Annex DAnionic active ingredient (wt %)

    a12 - ISO 2271: 1989

    Total mixed active ingredientdetergent

    b

    12 -

    - anionic active ingredient (wt %) 8 - ISO 2271: 1989

    - other active ingredientc

    (wt %) 1.5 -

    (ISO 2871-1: 1988 andISO 2871-2: 1990)

    d

    and/or BS 3762-3.7:1986)

    e

    Phosphates as P2O5 (wt %) - 20 ISO 4313: 1976

    Sodium silicates (as SiO2) (wt %) 5 12 ISO 8215: 1985

    Sodium carboxymethylcellulose(wt %)

    f

    0.2 - BS 3762-3.15: 1985

    Biodegradability of alkylbenzenesulphonate (where applicable)(% surfactant reduction)

    80 - ASTM D 2667-89

    Particle size

    Material passing through a US

    standard #10 (2000 m) sieve (wt%)

    100 -

    Material passing through a US

    standard #200 (75 m) sieve (wt

    %)

    - 3

    Procedure as detailed inASTM D 502-89 exceptuse US #10 and US #200

    standard sieves

    aThis applies if only anionic surfactants are used.

    bThe minimum amounts of anionic and other active ingredients are specified, and add up to 9.5 %. The total minimum amount

    of mixed active ingredient shall be 12 %, the remaining 2.5 % being either anionic or other active ingredient.c

    Other active ingredients are cationic and/or non-ionic active ingredient. dThe total cationic active ingredient (wt %) is equal to the sum total of the cationic active ingredient value (wt %) obtained from

    both ISO 2871-1: 1989 and ISO 2871-2: 1989.eBS 3762-3.7:1986 is used to determine the wt % for non-ionic active ingredient only.

    fThis applies if sodium carboxymethylcellulose is the only anti-redeposition agent used.

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    5 Test methods

    Tests for compliance with the specified limits for properties listed in Table 1 shall be carried out in

    accordance with the method specified for each property in Table 1. Compliance with the requirementspecified in clause 4.1.4 shall be determined by the test method described in Annex E.

    6 Sampling

    6.1 Sample size

    Each lot shall be tested separately for compliance with the requirements of this standard. The number(n) of primary packages to be selected to constitute a representative sample of the lot shall depend onthe size of the lot (N). The sample size for each lot shall be in accordance with Table 2.

    Table 2 Scale of sampling

    Lot or batch size, N

    (# of primary packages)

    Sample size, n

    (# of primary packages)

    2 - 25 2

    26 - 150 3

    151 - 1200 5

    1201 - 35000 8

    35001 and over 13

    NOTE The sample and lot sizes above were determined using Tables 1 and 2-A of ISO 2859-1:1999 Sampling procedures by attributes - Part 1: Sampling schemes indexed by acceptance quality limit (AQL) for lot-by-lot inspection. This applies to a single sampling plan for normal inspection and a special inspection level of S-2.

    6.2 Selection of primary packages

    The primary packages shall be selected systematically as described in 6.2.1 or randomly usingrandom number tables.

    6.2.1 Starting from any package, count and number all the primary packages in numerical order as1, 2, 3, 4 up to r(defined below), and withdraw every r

    thpackage thus counted to give a sample

    for the test.

    Where r= integral part ofN/nN= the lot or batch sizen = the number of primary packages to be selected (sample size)

    6.2.2 Where primary packages are grouped into secondary packages, as far as it is possible, onlyone package from each outer case shall be selected until the entire sample has been collected. Everyeffort shall be made to collect sample primary packages representative of all packing positions in the

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    secondary packages. The selection of secondary packages for the sampling exercise shall be carriedout in accordance with 6.3.

    6.3 Selection of secondary packages

    6.3.1 Where the number of secondary packages exceeds the sample size (n), secondary packageswill be selected randomly for inclusion in the sampling exercise.

    6.3.2 Where the sample size (n) exceeds the number of secondary packages, every effort shall bemade to apportion sampling quotas equally among the secondary packages of the lot.

    7 Conformity to requirements

    7.1 Lot conformity

    The entire lot shall be deemed as conforming to the requirements of this standard when the samplestaken in accordance with clauses 6.2 and 6.3 conform to the chemical and physical requirementsspecified in Table 1.

    7.2 Conformity assessment

    7.2.1 For each property to be tested on the individual samples of the lot, the mean ( x ) value and

    the range (R) value shall be calculated as follows:

    Mean ( x ) = Sum of test results

    Number of primary packages sampled

    Range (R) = The difference between the maximum and minimum values of the test results

    7.2.2 The samples shall be deemed as conforming to a particular chemical or physical requirementunder the following conditions:

    a) if the value of the expression ( Rx 4.0 ) is greater than or equal to the minimum value specifiedfor the property in Table 1, for which only the minimum value is given;

    b) if the value of the expression ( Rx 4.0+ ) is less than or equal to the maximum value givenspecified for the property in Table 1, for which only the maximum value is given; or

    c) if the value of the expression ( Rx 4.0 ) falls within the range of values specified for the property

    in Table 1, for which both the maximum and minimum values are given.

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    8 Packaging and labelling

    8.1 The detergent shall be packed in securely closed packages to ensure that the performance of

    the detergent is not affected and to prevent leakage.

    8.2 Packages for individual sale shall be conspicuously and legibly labelled and/or marked toconvey the following information:

    a) the name of the product which includes the words "laundry," "detergent," and "powder" or"powdered";

    EXAMPLE The name may be "powdered laundry detergent" or "laundry detergent powder".

    b) the brand name of the product and/or recognized trade mark, where applicable;

    c) the name and address of the manufacturer and/or distributor;

    d) the country of origin;

    e) the net weight of the contents of the packaged product in SIunits;

    f) instructions for applicable usage;

    g) precautions for use or potential hazards presented by product use;

    h) the month and year of manufacture;

    i) a "best before" date;

    j) the batch number or lot number stated in code or otherwise; and

    k) a caution statement as to the irritant capability of the detergent.

    EXAMPLE Detergent solution can be a skin irritant. Avoid prolonged contact. Rinse garment and handsthoroughly.

    l) first aid instructions, in the event of contact, inhalation, absorption, ingestion, fire, spillage orleakage of packages.

    NOTE Where the product has been certified by the Trinidad & Tobago Bureau of Standards, it may alsobear the TTBS standard mark.

    8.3 Labelling shall also comply with the requirements of TTS 76: Part 15, Requirements forLabelling Labelling of general household and automotive cleaning chemicals.

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    Annex A(normative)

    Determination of moisture and volatile matter content

    A.1 Apparatus

    a) Desiccators

    b) Oven capable of maintaining 105 C

    c) Petri dish

    d) Analytical balance (accuracy of 0.05 g)

    A.2 Procedure

    a) Weigh 10 g 0.1 g of detergent into a previously weighed Petri dish.

    b) Dry in an oven at 105 C 5 C for two hours.

    c) Cool in a desiccator and weigh.

    d) Continue heating, cooling and weighing until a constant weight is obtained.

    A.3 Calculation

    % moisture and volatile matter in sample = 100 x m/M

    Where m = mass of Petri dish & original sample mass of Petri dish & dried sample

    M= mass of original sample

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    Annex B(normative)

    Determination of pH value

    B.1 Apparatus

    a) pH meter:A standard pH meter which meets the requirements of BS 3145: 1978, Specificationfor laboratory pH meters

    b) Volumetric flask: 1000 ml capacity

    c) Beaker: 100 ml capacity

    d) Analytical balance (accuracy of 0.0005 g)

    B.2 Reagents

    a) Distilled water

    b) Standard buffer solution: Any suitable buffer solutions within the pH range of 9 to 11 units forcalibrating the pH meter

    B.3 Procedure

    a) Ensure that the pH meter is calibrated with standard buffer solutions before use (see also parts 1& 2 of BS 1647,pH measurement).

    b) Weigh 10 g 0.001 g of the material and transfer to a 1 L volumetric flask.

    c) Partially fill the flask with distilled water, stopper tightly and agitate until the sample is completelydissolved.

    d) Adjust the temperature of the solution and the distilled water to 27 C 0.5 C, and fill to thecalibration mark with the distilled water.

    e) Stopper the flask, mix thoroughly and allow the solution to stand at a temperature of 27 C for twohours prior to reading the pH value.

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    Annex C(normative)

    Determination of matter insoluble in water

    C.1 Apparatus

    a) Desiccator

    b) Beaker, capacity 250 ml

    c) Steam bath

    d) Buchner crucible

    e) Erlenmeyer filter flask

    f) Watch glass

    g) Oven capable of maintaining 105 C 5 C

    h) Analytical balance (accuracy of 0.005 g)

    C.2 Reagent

    Ethyl alcohol Freshly boiled, reagent grade, 95 % or higher, neutral to phenolphthalein

    C.3 Procedure

    a) Weigh 2 g to 10 g 0.01 g of the sample into a 250 ml beaker.

    b) Digest the sample with 200 ml of freshly boiled ethyl alcohol in a covered vessel on a steam bathuntil the soap is dissolved.

    c) Filter through a weighed Buchner crucible with suction, protecting the solution from carbondioxide and other acid fumes during the operation by covering with a watch glass.

    d) Wash the residue in the crucible with hot neutral ethyl alcohol until free from soap. Reserve thefiltrate and washings.

    e) After filtering and thoroughly washing the residue, change the receiver. Extract the residue withwater at 100

    C and wash the residue thoroughly.

    f) Dry the crucible and residue at 100 C to 105 C for three hours. Cool and weigh the matterinsoluble in water.

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    C.4 Calculation

    Matter insoluble in water, percent by mass = 100 x m/M

    Where m = mass in g of dried Buchner crucible & residue mass in g of empty Buchner crucible

    M= mass in g of the sample taken for the test.

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    Annex D(normative)

    Determination of free alkali as NaOH

    D.1 Apparatus

    a) Bunsen burner or hot plate

    b) Erlenmeyer flask

    c) Burette

    d) Analytical balance (accuracy of 0.005 g)

    D.2 Reagents

    a) Phenolphthalein indicator 1 % solution

    b) Hydrochloric acid standard 0.1 N

    D.3 Procedure

    a) Heat the reserved filtrate and washings to incipient boiling [see clause c.3 (d)].

    b) Add 0.5 ml of a 1 % solution of phenolphthalein.

    c) Titrate with standard 0.1 N HCl solution and calculate the free alkali as sodium hydroxide(NaOH).

    D.4 Calculation

    Free alkali as NaOH (% by mass) = 40 x 0.1 Vx 100M

    Where V= volume in ml of HCl used in titration

    M= mass in g of the sample taken for the test (from annex C).

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    Annex E(normative)

    Determination of net weight of product

    E.1 Apparatus

    a) Top-loading balance (accurate to 0.05 g)

    b) Container capable of holding the contents of the package of detergent

    E.2 Procedure

    a) Weigh the empty container.

    b) Empty as much of the contents of the package into the container and record the weight.

    E.3 Calculation

    The average of the difference in weight shall be taken as the net weight per package.

    Net weight = mass in g of container & contents mass in g of empty container

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    Annex F(informative)

    Additional commonly used detergent ingredients

    The following is a list of additional commonly used detergent ingredients:

    a) Corrosion inhibitors

    b) Fluorescent whitening agents

    c) Processing aids

    d) Colorants

    e) Fragrances

    f) Oxygen bleach

    g) Enzymes

    h) Suds control agents

    i) Fabric softening agents

    j) Other ingredients which provide specialized performance or convenience