ÿþ<html> <head> <meta http-equiv="Content-Language" content="en-us"> <meta http-equiv="Content-Type" content="text/html; charset=utf-8"> <meta http-equiv="Content-Type" content="text/html; charset=UTF-8"> <title> :: Acts And Rules :: </title> <meta http-equiv="Content-Type" content="text/html; charset=windows-1252"> <meta name="keywords" content="Publication, Shetkari magzin, Litereture , Shetishastra,Agriculture Portal, Maharashtra Government, employment, law and acts "> <META NAME="description" CONTENT="This is the Portal of Agriculture Department of Maharshtra State (India), developed with an objective to enable a single window access to information and services being provided by Agriculture Department."> <Script language="JavaScript"> var Txt = "Welcome to mahaagri.gov.in (Department of Agriculture ,Government of Maharashtra)"; var space = " "; var A =0; function MessageInStatus() { window.status = Txt.substring(A, Txt.length) + space + Txt.substring(0, A); A ++; if (A > Txt.length) A = 0; window.setTimeout("MessageInStatus()", 200); } MessageInStatus(); </Script> <style type="text/css"> <!-- body { margin-left: 1px; margin-top: 0px; margin-right: 0px; margin-bottom: 0px; font-family: verdana; font-size: 11px; color: #000000; scrollbar-face-color: #BBD5BF; scrollbar-highlight-color: White; scrollbar-shadow-color: White; scrollbar-3dlight-color: #FFFFFF; scrollbar-arrow-color: Green; scrollbar-track-color: #D9FED3; scrollbar-darkshadow-color: Green } a:link { text-decoration: none; } a:visited { text-decoration: none; } a:hover { text-decoration: underline; font-weight: bold; color: Blue; } a:active { text-decoration: none; } .headingm { font-family: arial; font-size: 13px; color: #355313; padding-left: 5px; } table.MsoNormalTable {mso-style-parent:""; font-size:10.0pt; font-family:"Times New Roman" } table.MsoTableGrid {border:1.0pt solid windowtext; font-size:10.0pt; font-family:"Times New Roman"; } li.MsoNormal {mso-style-parent:""; margin-bottom:.0001pt; font-size:12.0pt; font-family:"Times New Roman"; margin-left:0in; margin-right:0in; margin-top:0in} ----> </style> </head> <body bgcolor="#EFEFEF" > <table id="Table_01" width="1" height="1" border="0" cellpadding="0" cellspacing="0"> <tr> <td rowspan="2" height="1" width="168" bgcolor="#536A45"> <p style="margin-top: 0; margin-bottom: 0" dir="ltr"> <img src="../images/InnerIndex_01.gif" width="168" height="169" alt=""></td> <td colspan="3" height="90" width="838" bgcolor="#536A45"> <p style="margin-top: 0; margin-bottom: 0"> <img src="../images/InnerIndex_02.gif" width="833" height="97" alt=""></td> </tr> <tr> <td height="1" width="63"> <p style="margin-top: 0; margin-bottom: 0"> <img src="../images/InnerIndex_03.gif" width="63" height="72" alt=""></td> <td height="1" width="705"> <table border="0" cellpadding="0" cellspacing="0" style="border-collapse: collapse" bordercolor="#111111" width="100%" id="AutoNumber3" height="28"> <tr> <td width="100%" bgcolor="#9AD7ED" height="28" dir="ltr"> <p style="margin-left: 55; margin-top:0; margin-bottom:0"><font color="#882E0F"><b><font color="#882E0F"> <font face="Verdana" color="#008000" size="2">The Fertilizer (Control), Order 1985</font></font></b></font ></td> </tr> </table> </td> <td height="1" width="84" background="../images/InnerIndex_05.gif"> <table border="0" cellpadding="0" cellspacing="0" style="border-collapse: collapse" bordercolor="#111111" width="80%" id="AutoNumber4" height="29"> <tr> <td width="26%" bgcolor="#9AD7ED" height="29" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="9%" height="29" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="18%" bgcolor="#9AD7ED" height="29" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="3%" height="29"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="14%" bgcolor="#9AD7ED" height="29"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="5%" height="29"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="11%" bgcolor="#9AD7ED" height="29"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="11%" height="29"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="5%" bgcolor="#9AD7ED" height="29"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> </tr> </table> </td> </tr> </table> <table border="0" cellpadding="0" cellspacing="0" style="border-collapse: collapse" bordercolor="#111111" width="99%" id="AutoNumber1" height="393"> <tr> <td width="100%" height="393"> <table border="0" cellpadding="0" cellspacing="0" style="border-collapse: collapse" bordercolor="#111111" width="99%" id="AutoNumber2" height="1"> <tr> <td width="17%" height="1" bgcolor="#536A45" valign="top"> <table border="0" cellpadding="0" cellspacing="0" style="border-collapse: collapse" bordercolor="#111111" width="100%" id="AutoNumber7" height="427"> <tr> <td width="100%" height="427" valign="top"> <table border="0" cellpadding="2" style="border-collapse: collapse" bordercolor="#111111" width="100%" id="AutoNumber8" height="265"> <tr> <td width="6%" bgcolor="#C7D6BE" height="21" align="right" style="border-style: none; border-width: medium" dir="ltr"> <p dir="ltr" style="margin-top: 0; margin-bottom: 0"> <img border="0" src="../images/Mag.gif" width="4" height="7"></td> <td width="94%" bgcolor="#C7D6BE" height="18" style="border-style: none; border-width: medium" dir="ltr"> <p style="margin-left: 5; margin-top:0; margin-bottom:0"class="headingm" dir="ltr"><span dir="LTR"><strong> <span style="font-weight:normal"> <a href="Frt_Order_1973.html">Fertilizer Control Order, 1973</a></span></strong></span></td> </tr> <tr> <td width="6%" height="18" align="right" style="border-top-style: none; border-top-width: medium" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> <td width="94%" height="18" style="border-top-style: none; border-top-width: medium" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> </tr> <tr> <td width="6%" bgcolor="#C7D6BE" height="21" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"> <img border="0" src="../images/Mag.gif" width="4" height="7"></td> <td width="94%" bgcolor="#C7D6BE" height="21" dir="ltr"> &nbsp;</td> </tr> <tr> <td width="6%" height="18" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> <td width="94%" height="18" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> </tr> <tr> <td width="6%" bgcolor="#C7D6BE" height="22" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"> <img border="0" src="../images/Mag.gif" width="4" height="7"></td> <td width="94%" bgcolor="#C7D6BE" height="22" dir="ltr"> &nbsp;</td> </tr> <tr> <td width="6%" height="18" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> <td width="94%" height="18" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> </tr> <tr> <td width="6%" bgcolor="#C7D6BE" height="22" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"> &nbsp;</td> <td width="94%" bgcolor="#C7D6BE" height="22" dir="ltr"> <p align="center">&nbsp;</td> </tr> <tr> <td width="6%" height="20" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> <td width="94%" height="20" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> </tr> <tr> <td width="6%" bgcolor="#C7D6BE" height="22" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"> <img border="0" src="../images/Mag.gif" width="4" height="7"></td> <td width="94%" bgcolor="#C7D6BE" height="22" dir="ltr"> &nbsp;</td> </tr> <tr> <td width="6%" height="19" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> <td width="94%" height="19" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> </tr> <tr> <td width="6%" bgcolor="#C7D6BE" height="22" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"> <img border="0" src="../images/Mag.gif" width="4" height="7"></td> <td width="94%" bgcolor="#C7D6BE" height="22" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> </tr> <tr> <td width="6%" height="18" align="right" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> <td width="94%" height="18" dir="ltr"> <p style="margin-top: 0; margin-bottom: 0"></td> </tr> </table> </td> </tr> </table> </td> <td width="83%" height="1" valign="top" align="center"> <table border="0" cellpadding="0" cellspacing="0" style="border-collapse: collapse" bordercolor="#111111" width="100%" id="AutoNumber5"> <tr> <td width="100%"> <table border="0" cellpadding="0" cellspacing="0" style="border-collapse: collapse" width="99%" id="AutoNumber6" height="24"> <tr> <td width="8%" height="291"> <p style="margin-top: 0; margin-bottom: 0">&nbsp;</td> <td width="92%" height="291"> <p class="MsoNormal" align="center" style="margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2" color="#CF4516">SCHEDULE II<a name="sII"> </a></font></span></font></b></p> <p class="MsoNormal" align="center" style="margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF; font-weight:700"> <font size="2" color="#882E0F">(See clause 28 (1) (b) and 29)</font></span></p> <p class="MsoNormal" align="center" style="text-align: justify; margin-top: 0; margin-bottom: 0">&nbsp;</p> <p class="MsoNormal" align="center" style="margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">PART A<a name="pa"> </a></font></span></font></b></p> <p class="MsoNormal" align="center" style="margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">PROCEDURE FOR DRAWAL OF SAMPLES OF FERTILIZERS</font></span></font></b></p> <p class="MsoNormal" align="center" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">1. General requirement of sampling</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">In drawing samples, the following measures and precautions </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">should be observed.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Samples shall not be taken at a place exposed to rain/sun;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) The sampling instruments shall be clean and dry when used;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) The material being sampled, the sampling instrument and the bags of samples should be free from any adventitious contaminations;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) To draw a representative sample, the contents of each bag selected for sampling should be mixed as thoroughly as possible by suitable means;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) The sample should be kept in suitable, clean dry and air tight glass or screwed hard polythene bottle of about 400 gm capacity or in a thick gauged polythene bag. This should be put in a cloth bag which may be sealed with the Inspector&#39;s seal after putting inside the detailed description as specified in Form &quot;J&quot; Identifiable details may also be put on the cloth bag like sample No./Code No. or any other details which enables its identification; </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(f) Each sample bag should be sealed air tight after filling and marked with details of sample, type and brand of fertilizer, name of dealer/manufacturer/importer and the name of Inspector who has collected sample. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">2. Sampling from bagged material</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Scale of sampling</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Lot (for manufacturers/importers)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">All bags in a single consignment of the material of the same grade and type drawn from a single batch of the manufacturer/importer shall constitute a lot. If a consignment is declared to consist of different batches of manufacturer/import, all the bags of each batch shall constitute a separate lot. In the case of a consignment drawn from a continuous process,2000 bags (or 100 tones) of the material shall constitute a lot.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Lot (for dealers)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">The lot is an identifiable quantity of same grade and type of fertilizer stored at an identifiable place subject to a maximum limit of 100 tones. The lot shall be identified by the inspector based on visible appearance of bags, their packing and storage conditions. The stock of less than 100 tones with a dealer may also constitute one or more lots, if the material (fertilizer) of different sources and brand is available in such quantities. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Selection of bags for sampling </font></span> </p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">The number of bags to be chosen from a lot shall depend upon the size of the lot as given in the table below.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <table class="MsoNormalTable" border="1" cellspacing="0" cellpadding="0" width="423" style="width: 317.25pt; border: 1.0pt solid windowtext"> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">Lot size (No. of bags) (N)</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">No. of bags to be selected for sampling (n)</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">Less than 10</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">1</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 10-100</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">2</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 100-200</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">3</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 200-400</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">4</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 400-600</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">5</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 600-800</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">6</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 800-1000</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">7</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 1000-1300</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">8</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 1300-1600</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">9</span></td> </tr> <tr> <td width="47%" valign="top" style="width: 47.04%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> 1600-2000</span></td> <td width="52%" valign="top" style="width: 52.96%; border: 1.0pt solid windowtext; padding: 5.25pt"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">10</span></td> </tr> </table> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">All the bags of a lot should be arranged in a systematic manner. Start counting from any bag randomly, go on counting as 1,2,3,- up to r and so on, r being equal to the integral of N/n. Thus every rth bag counted shall be withdrawn and all bags shall constitute the sample bags from where the sample is to be drawn for preparing a composite sample.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) Sampling from big godowns/high stackings.</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">If the procedure given in Para 2(i) (c) is not possible to be adopted, the sample should be drawn from the randomly selected fertilizer bags from different layers, from top and from all open side in a zig fashion.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iii) Sampling from small godowns</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">All the fertilizer bags of the same grade and type of each manufacturer though received on different dates shall be segregated and properly stacked. All bags of same grade and type of fertilizer manufactured by a particular manufacturing unit may be considered as one lot based on their physical conditions and the sample shall be drawn as per procedure laid in Para 2(i) (c) and 4.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iv) Sampling from damaged stock</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) In case of torn or lumpy bags, damaged fertilizer bags or sweepings, the stock should be arranged according to identifiable lots. From each lot the number of bags shall be selected as per procedure 2(i)(c). If the bags allow the use of sampling probe conveniently, the samples should be drawn by sampling probe.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) In case it is not possible to use the sampling probe, the bags may be opened and fertilizer material mixed together uniformly by hammering the big lumps or putting pressure, if required and then samples drawn by using suitable sample device. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">3. Sampling probe</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) An appropriate sampling instrument to be used by the Inspectors for collection of a representative sample is called sampling probe. The probe may comprise of a slotted single tube with soil cone tip made of stainless steel or brass. The length of the probe may be approximately 60 to 65 cms and the diameter of the tube may be approximately 1.5 cm and the slot width 1.2 to 1.3 cms. The probe may be use if the physical condition of the fertilizers and the packing material permits it use.&nbsp; </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) In case of High Density Polyethylene packing and also when the fertilizer material is not in free flowing condition, the use of sampling probe may not be possible. In such a case, selected bags for drawing samples may be opened and the fertilizers may be taken out of the bags and spread on a clean surface and samples drawn with the help of a suitable Sampling device which may be made of stainless steel or brass cup.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">4. Drawal of samples from bags.</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Drawal of sample and preparation of composite samples. Draw, with an appropriate sampling instrument, (sampling probe) small portions of the material from the selected bags as per procedure in para 2(i) (b) 2(ii) 2(iii)and 2 (iv) (a). The sampling probe shall be inserted in the bag from one corner to another diagonally and when filled with fertilizer, the probe is withdrawn and fertilizer is emptied in a container/or on polythene sheet/or on a clean hard surface and made into one composite sample.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) If the bags do not permit the use of sampling probe, empty the contents of the bags on a level, clean and hard surface and draw a composite sample by the process of quartering as described under para 3 (ii) or 5.+(iii) In case of chelated micro-nutrients and mixtures of micro-nutrients, the three identical containers of the batch, grade, type and manufacturer, shall be selected which shall constitute the composite samples, provided it is not possible to draw a composite sample of the size given under para 4A (iii).&quot;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&quot;4A. Weight of one sample</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">One sample of fertilizer shall have the approximate weight, as specified below:-</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) For straight micro-nutrient fertilizers- 100gms.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) For chelated micro-nutrient fertilizers and 50gms or mixtures of micro-nutrients the maximum&nbsp; packing size of similar quantity</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iii) For other fertilizer and mixtures of fertilizers 400 gms.&quot;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">5. Preparation of composite sample</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">If the composite sample collected from the different selected bags is large than required weight, its size shall be reduced by method of quartering as detailed below:-</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Spread the composite sample on a level, clean, hard surface, flatten it out and divide it into four equal parts. Remove any diagonally opposite parts. Mix the tow remaining parts together to form a cone, flatten out the cone and repeat the operation of quartering till a composite sample of required weight is obtained. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">6. Preparation of test sample and reference sample</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) The composite sample obtained above shall be spread out on a clean, hard surface and divided into three approximately equal proportions + each of the weight as specified in Para 4A. Each of these samples shall constitute the test sample. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) Each test sample shall be immediately transferred to a suitable container as defined under para 1(e). The slip with detailed description may be put inside the sample bag. Each bag shall also be properly labeled as mentioned in Para 1(f)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iii) Each test sample container shall then be sealed with the seals of the inspector. If possible, seal of the manufacturer/importer/dealer or purchaser as the case may be, may also be affixed.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iv) One sample so sealed shall be sent to the Incharge of the Laboratory notified by the State Government under clause 29 or Central Fertilizer Quality Control and Training institute, Faridabad * or Regional Fertilizer Control Laboratories at Bombay, Madras or Kalyani (Calcutta) for analysis and the second give to the manufacturer or importer or dealer or the purchaser as the case may be. The third sample shall constitute the reference sample and shall be sent by the inspector to his next higher authority for keeping in safe custody for production in court, if required.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">7. Sampling from the bulk fertilizers in ships, bulk carriers and bulk containers.</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Sampling equipments</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Sampling cup</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">The sampling cup can be fabricated from non-corrosive metal, Inside dimensions of cup mouth may be 3/4&quot; X 10&quot; as per he diagram of the sampling cup given in Figure -1.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Sampling probe for bulk fertilizers.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">The sampling probe should be made of non-corrodable material such as stainless steel or brass. It may be slotted double tube with solid cone tip having a length of about 4 1/2&#39;-5&#39; and diameter of about 1 1/4&quot; to 1 1/2&quot;.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(</font></span><span style="font-family: Verdana; background-color: #EFEFEF"><font size="2">c) Scoop</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Samples from the hatch can also be collected by suitable scoop made of stainless steel or brass. (Figure 1 - sampling cup)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) Sampling procedure</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Drawal of samples from the ship of bulk fertilizers</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A. Sampling from conveyor belt. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">When the material is unloaded from the ships transported to temporary/storage godowns through conveyor belts, the sample can be drawn by passing the sampling cup through the entire stream of material as the material drops from a transfer belt or spout. The long slot in the top of sampling cup should be perpendicular to the falling stream. pass the cup through the complete stream at a uniform speed, so that the cup will collect approximately equal amounts in each pass but will never overflow.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A minimum of 10 equally timed and speed stream must be taken during the transfer operation. However, the stream samples are not applicable unless uniform continuous flow of fertilizer is maintained for more than 3 minutes while lot is being sampled. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">B. Sampling from hatch.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">In case of bulk fertilizers, from each hatch, at least 5-6 composite samples should be drawn from different depths and different points during unloading operation. To make one composite sample, minimum 5 samples should be drawn from different points at a specific depth. All these samples should be mixed to make one composite sample. The depths may be 0-5 m,5-10m, 10-15m, 15-20 m and 20-25 m depending upon the depth of hatch. The samples at a particular depth should be drawn after removal of material up to the required depth. The samples may be drawn with the help of sampling probe or scoop.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Drawal of samples from bulk carriers-trucks etc. The sample can be drawn as per vertical probing procedure of Association of Official Analytical Chemists. The sampling probe should be about 4 1/2&#39; to 5&#39; length. Draw 10 Vertical cuts from the following locations relative to the entire top of the conveyance. The 10 vertical cores are combined into a composite sample. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <table class="MsoNormalTable" border="1" cellspacing="0" cellpadding="0" style="width: 382; border-collapse: collapse; border: medium none" height="57"> <tr> <td valign="top" style="width: 110; border: 1.0pt solid windowtext; padding: 5.25pt" height="30"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">7</span></td> <td colspan="2" valign="top" style="width: 152; border-left: medium none; border-right: 1.0pt solid windowtext; border-top: 1.0pt solid windowtext; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="30"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">4</span></td> <td valign="top" style="width: 74; border-left: medium none; border-right: 1.0pt solid windowtext; border-top: 1.0pt solid windowtext; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="30"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">8</span></td> </tr> <tr> <td valign="top" style="width: 110; border-left: 1.0pt solid windowtext; border-right: 1.0pt solid windowtext; border-top: medium none; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="29"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">3</span></td> <td valign="top" style="width: 73; border-left: medium none; border-right: 1.0pt solid windowtext; border-top: medium none; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="29"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">1</span></td> <td valign="top" style="width: 64; border-left: medium none; border-right: 1.0pt solid windowtext; border-top: medium none; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="29"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">2</span></td> <td valign="top" style="width: 74; border-left: medium none; border-right: 1.0pt solid windowtext; border-top: medium none; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="29"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">5</span></td> </tr> <tr> <td valign="top" style="width: 110; border-left: 1.0pt solid windowtext; border-right: 1.0pt solid windowtext; border-top: medium none; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="44"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">10</span></td> <td colspan="2" valign="top" style="width: 152; border-left: medium none; border-right: 1.0pt solid windowtext; border-top: medium none; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="44"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">6</span></td> <td valign="top" style="width: 74; border-left: medium none; border-right: 1.0pt solid windowtext; border-top: medium none; border-bottom: 1.0pt solid windowtext; padding: 5.25pt" height="44"> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF">9</span></td> </tr> <![if !supportMisalignedColumns]> <tr height="0"> <td width="126" style="border:none" height="1"> <p align="justify" style="margin-top: 0; margin-bottom: 0"> </td> <td width="88" style="border:none" height="1"> <p align="justify" style="margin-top: 0; margin-bottom: 0"> </td> <td width="79" style="border:none" height="1"> <p align="justify" style="margin-top: 0; margin-bottom: 0"> </td> <td width="89" style="border:none" height="1"> <p align="justify" style="margin-top: 0; margin-bottom: 0"> </td> </tr> <![endif]> </table> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Drawal of samples from bulk material in storage.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(A) The bulk storage piles (level or flat) up to 100 tones could be sampled as per Figure 2. Take 10 cores to the maximum possible depth of the probe from the position indicated in the Figure 2 and cores are composited.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(B) A one sided or slopped pile may be sampled at the points illustrated in Figure3. Withdraw one vertical core of material from location 1 &amp; 6 and two cores at locations 2, 3,4 &amp; 5 composite all the probe samples and prepare the composite sample for analysis as per procedure laid down in para 1,5 &amp; 6.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Figure 2- Sample points for coned or ridged pile)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">8. Method of sampling of anhydrous ammonia</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp; (i) Scope </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">This method is for use obtaining samples of anhydrous ammonia. The method is based on the assumption that the material to be sampled is as claimed and contains only a small amount of impurity primarily water. It is recommended that duplicate samples be taken form each tank or vessel sampled. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0">&nbsp;</p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) Apparatus</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Tubes for sampling tubes, heat resistant glass, conical centrifuge type 200ml with lower 100 ml graduated from 0.2 ml in 0.05 ml divisions, 2-4 ml in 0.1 division, 4-10 ml in 0.5 ml divisions and 10-100 ml in 1.0mldivisions. Tube type is shown in figure 5.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Stoppers for tubes, rubber, with bent tube vent as in Figures 5.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Samples carrier, constructed of plywood or aluminum as in Figure 5.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Sampling line and connection assembly constructed as in Figure 4, with flexible steel sampling nose 48&quot; long, 1/4&quot; NPT coupling at each end and 1/8&quot; insulated steel tubing delivery tip at one end. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) Sample tube adapter, constructed from rubber stopper and 6mm D. D. glass or steel tubing as in Figure 5.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(f) Protective equipment: Rubber or other non-porous gloves, offering complete protection to the hands lower arms, full coverage goggles or approved gas mask.( Figure 4)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp; (iii)Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Charcoal, reagent, 14-20 mesh.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Note: If the sample is expected to contain excessive amount of water (one percent or more) one piece of the charcoal may be added to each tube before introduction of the sample</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp; (iv) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Place two dry, clean sampling tubes in the sample carrier</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Connect the sampling line connection assembly to the unloading valve of the tank, vessel, or line to be sampled.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Open the valves slowly and purge the sampling line connection assembly thoroughly by venting 3 to 4 liters of ammonia. Close the sample line globe valve. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Remove the vented stoppers from the tubes and insert the adopter end of the sampling line connection assembly.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) Open the sample line valve and slowly fill the sampling tube to the100ml mark, close the sample line valve.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(f) Remove the sampling line adopter and insert the vented stopper in the sampling tube.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(g) Repeat steps, d, e, and f and fill the second tube. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(h) close tank discharge valve and remove the sampling line connection assembly. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Either know or note the vessel, container, or line pressure of material sampled.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(j) Tag the collected samples for identification and submit to the laboratory for processing by following methods in this section </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0">&nbsp;</p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp; (v) Precaution</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Liquid anhydrous ammonia causes severe burns on contact. It evaporates readily releasing the gas which may cause varying degrees of irritation of the skin and mucus membrane and may injure severely the respiratory mucosa with possible fatal outcome.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Avoid contacting liquid ammonia. In case of contact, immediately flush the affected parts with plenty of water for atleast 15 minutes. Get medical attention at once in case of burns, especially to the eyes, nose and throat, or if the victim is unconscious. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Ammonium gas in concentrations of 6,000 to 10,000 ppm (by volume) is lethal within a few minutes. Irrigation of the eyes, respiratory tract and throat results from concentrations as low as 500 to 1,000 ppm&#39; a concentration of 2,000 ppm produces convulsive coughing and may be fatal after a short exposure i.e. less than half an hour. The maximum concentration tolerated by the skin for more than few seconds is 2 percent (i.e. when suitable respiratory protection is worm) The maximum allowable concentration for 8 hour working exposure is 50 ppm. This is the least detectable order. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Obtain medical attention if exposure to the gas produce distress of any type.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) Rubber or other no porous gloves, offering complete protection to the hands and lower arms must also be worn to protect the eyes unless an approved gas mask is used. The gas mask need only to be used if sampling can not be done without possible inhalation of the vapours. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0">&nbsp;</p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0">&nbsp;</p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0">&nbsp;</p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" align="center" style="margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">PART B<a name="pb"> </a></font></span></font></b></p> <p class="MsoNormal" align="center" style="margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; font-weight: 700; background: #EFEFEF"> <font size="2" color="#882E0F">METHOD OF ANALYSIS OF FERTILIZERS</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0">&nbsp;</p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">1. Preparation of sample for analysis in the laboratory</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reduce gross sample to quantity sufficient for analysis or grind not &lt; 250 Gm of reduced sample without previous sieving.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) For fertilizer materials and moist fertilizer mixtures, that form a paste on putting pressure, grind in porcelain pestle and mortar to pass sieve with 1mm circular openings or No. 20 standard sieve. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) For dry mixtures that tend to segregate, grind in a porcelain pestle and mortar to pass No. 40 standard sieve.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Grind as rapidly as possible to a avoid loss or gain of moisture during operation.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) Mix thoroughly and store in tightly stoppered bottles.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">2. Determination of moisture</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Not applicable to samples that yield volatile substances other than water at drying temperature)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Weight to the nearest mg about 2gm of the prepared sample in a weighed, clean, dry squat form weighing bottle. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Heat in an oven for about 5 hours at 99-101 C to constant weight Cool in a desicator and weigh.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) In case of sodium nitrate ammonium sulphate and potassium salts heat to constant weight at 129-131 C</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Report percentage loss in weight as moisture at temperature used.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">100(B-C)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Free moisture percent by weight = 100(B-C)/B-A</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A= Weight of the bottle</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">B= Weight of bottle plus material before drying.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">C= Weight of the bottle plus material after drying. (Reference - Methods of analysis. AOAC 1965) </font> </span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) Moisture in ammonium chloride </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Weigh accurately about 5gm of prepared sample in a weighed shallow porcelain dish and dry for 24 hours in a vacuum desicator over sulphuric acid and re-weight. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Preserve the dried material for subsequent tests.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Moisture percent by weight = 100 x W<sub>1</sub>/W</font><sub><font size="2">3</font></sub></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">W<sub>1</sub>= loss in weight in gm on drying and </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">W<sub>3</sub>= Weight in gm of the prepared sample taken for the test. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iii) Samples like urea, diammonium phosphate and ammonium nitrate which yield volatile substances other than water at drying temperature. the Karl Fischer method given below is use for the determination of moisture.</font></span><span style="font-family: Verdana; background-color: #EFEFEF"><font size="2"> </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iv) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Iodine solution -add 125 gm of iodine to a mixture of 650 ml of methanol and 200 ml of pyridine contained in a flask, and immediately close the flask tightly.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Sulphur dioxide solution-pass dry sulphur dioxide into 100 ml of pyridine contained in a 250 ml graduated cylinder and cooled in an ice bath, until the volume reaches 200 ml. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Fisher Reagent- Slowly add iodine solution to the cooled sulphur dioxide solution stopper immediately and shake well until the iodine is dissolved. Transfer the solution to an automatic pipette, protected from absorption of moisture by a drying agent and allow to stand for 24 hours before standardizing. The reagent deteriorates continuously and it should be standardized within one hour before use.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(v) Procedure </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Determination of end point in Karl Fischer Titration- In many cases, the end point can be detected visually by the change of colour </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Sulphur dioxide solution -pass dry sulphur dioxide into to 100 ml of pyridine contained in a 250 ml graduated cylinder and cooled in an ice bath, until the volume reaches 200 ml.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Fisher reagent-Slowly add iodine solution to the cooled sulphur dioxide solution stopper immediately and shake well until the iodine is dissolved. Transfer the solution of moisture by a drying agent and allow to stand for 24 hours before standardizing. The reagent deteriorates continuously and it should be standardized within one hour before use. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Standard water solution- Measure exactly 2ml of water into a thoroughly dry 1 liter volumetric flask, dilute to volume with methanol. retain sufficient quantity of the same methanol for blank determination. Keep the solution in tightly closed containers. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(vi) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Determination of end point in Karl Fischer Titration- In many cases, the end point can be detected visually by the change of colour from a light brownish yellow to amber. But when the end point is not clearly defined, the electrometric method for determining the end point should be adopted. Adjust the potentiometer so that when a small excess 90.02 ml) of the reagent is present a current of 50 to 150 microampers is recorded. The solution should be continuously and vigorously stirred. At the beginning of the titration, a current of only a few microampers will flow. After each addition of regent, the pointer of the micrometer deflected but rapidly returns to the original position. At the end point deflection is obtained which endures for a longer period.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Standardization of the Fischer reagent-Pipette exactly 10ml or methanol into a dry titration flask and titrate with the Fischer reagent to the end point (V<sub>1</sub>) Pipette exactly 10ml of the standard water solution into the flask and titrate to the end point (V<sub>2</sub>). </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Titration of the material-Transfer 25ml. of methanol to the titration flask and titrate to the end point (V<sub>3</sub>) with the Fischer reagent. Do not record the volume consumed. Quickly transfer to the titrated liquid an accurately weighed quantity of the material containing 10 to 50 mg. of water, stir vigorously and titrate to the end point. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculation</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Moisture percent by weight = 0.1 x W(V<sub>3</sub> ýÿ 2.5V<sub>1</sub>) / (V<sub>2</sub>- V<sub>1</sub>)A </font> </span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Where W= Weight in mg. of water contained in 10ml of standard </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">water solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">V<sub>3</sub>= Total volume in ml of the reagent use in titration in (c)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">V<sub>1</sub>= Volume in ml of reagent used in titration of methanol in(b)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">V<sub>2</sub>= Total volume in ml of the reagent use in titration in (b)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A= Weight in gm. of the material taken for the test in (C)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference- I.S. Specification for urea. technical and pure I.S. 1781-1961)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">3. Determination of nitrogen</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Methods of determination of total nitrogen have been described separately in this section. These methods can be adopted both for straight and mixed fertilizers. Scope of each method with various combinations have also been described with each method.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">The relevant methods of analysis which have been described are as given below:</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Total nitrogen--for nitrate free samples.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Total nitrogen--for nitrate containing samples.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Total nitrogen--for materials with high Cl: No3 ration and to materials containing only water soluble nitrogen.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Total nitrogen--for nitrate free samples.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Determination of ammoniacal nitrogen.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) Determination of ammoniacal and nitrate nitrogen.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(f) Determination of nitrate nitrogen. </font> </span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(g) Determination of water insoluble nitrogen. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(h) Determination of urea nitrogen. </font> </span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Detection of nitrate</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">For adopting a specific method as described above, it is necessary to detect the presence of nitrates in the sample before a particular method is adopted. The procedure for detection of nitrates is given below:-</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Mix 5gm sample with 25ml hot water and filter.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) To one volume of this solution add 2 volume of sulphuric acid, free from HNO<sub>3</sub> and oxides of N and let it cool.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Add a few drops of concentrated FesO<sub>4</sub> solution in such a manner that fluids do not mix. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) If the nitrates are present junction shows at first purple, afterward brown, or if only minute quantity is present, reddish colour. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) To another portion of solution add 1ml. 1 percent Na NO<sub>3</sub> and test as before to determine whether enough H<sub>2</sub>SO<sub>4 </sub>was added in the first test. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference -methods of analysis. AOAC 1965)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) Reagents for determination of total nitrogen</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Sulphuric acid - 93-98 percent H<sub>2</sub>SO<sub>4</sub> N free.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Copper sulphate - Cu SO<sub>4</sub>5H<sub>2</sub>O reagent grade. N free.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Potassium sulphate (or anhydrous sodium sulphate)-reagent grade.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Salicylic acid- reagent grade, N free</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) Sulphide or the sulphate solution- Dissolve 40 gm. commercial K2S in liter distilled water.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Solution- of 40gm Na<sub>2</sub>S or 80gm Na<sub>2</sub>S<sub>2</sub>O<sub>3</sub>.5H<sub>2</sub>O in 1 liter may be use)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(f) Sodium hydroxide- pellets or solution, nitrate free. for solution dissolve approximately 450 gm solid NaOH in distilled water and dilute to 1 liter (Sq. gr. of solution should be 1.36 or higher)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(g) Zinc granule-- reagent grade.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(h) Zinc dust-- Impalpable powder.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Methyl red indicator- Dissolve 1gm. methyl red in 200 ml. alcohol. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(j) Hydrochloric or sulphuric acid standard solution,--0.5 N or 0.1 N when amount or N is small. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(k) Sodium hydroxide standard solution-- 0.1 N(or other specified concentration)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Standardize each standard solution with primary standard and check one against another. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Test reagents before using, by blank determination with 2 gm. sugar which insures partial reduction of any nitrates present. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Caution:</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Use freshly opened sulphuric acid or add dry P<sub>2</sub>O<sub>5</sub> to avoid hydrolysis of nitrites and cyanates. Ratio of salt to acid (wt: Vol) should be approximately 1:1 at end of digestion for proper temperature control. Digestion may be incomplete at lower ration, N may be lost at higher ration. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iii) Apparatus</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) For digestion-- Use Kjeldahl flask of hard moderately thick, well annealed glass with total capacity approximately 500-800 ml. Conduct digestion over heating device, adjusted to bring 250 ml. water at 25C to rolling boil in a approximately for 5 minutes. Add 3-4 boiling chips to prevent superheating. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) For distillation- Use Kjeldahl or other suitable flask of 500--800 ml. capacity filled with rubber stopper through which passes. lower end of efficient scrubber bulb or trap to prevent mechanical carryover of NaOH during distillation. Connect upper end of bulb tube to condenser tube by rubber tubing. Trap outlet of condenser in such a way as to insure complete absorption of ammonia distilled over into acid in receiver. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iv) Total nitrogen (in nitrate free samples)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Place weighed sample (0.7-2.2gm.) in digestion flask.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Add 0.7 gm. copper sulphate, 15 gm. powdered K<sub>2</sub>SO<sub>4 </sub>at anhydrous Na<sub>2</sub> SO<sub>4</sub> and 25ml.H<sub> 2</sub>SO</font><sub><font size="2">4</font></sub></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) If sample more than2.2 gm. is used, increase sulphuric acid by 10 ml. for each gm. sample. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Place flask in inclined position and heat gently until frothing ceases (if necessary add small amount of paraffin to reduce frothing)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Boil briskly until solution clears and then for at least 30 minutes longer (2 hours for sample containing organic material).</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Cool add approximately 200ml. distilled. water, cool below 25C. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) Add to the flask a layer of sodium hydroxide (25 gm. solid reagent or enough solution to make contents strongly alkaline ) without agitation. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Immediately connect flask to distilling bulb or condenser and with tip of condenser immerse in standard acid in receiver. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(9) Rotate flask to mix contents thoroughly, then heat until all amonia has distilled (a least 150 ml. distillate)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(10) Titrate excess standard acid in distillate with standard sodium hydroxide solution, using methyl red as an indicator. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(11) Correct for blank determination on reagents. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculation</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Percent nitrogen =(A Na-BNb)x0.01401 x 100 / W</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A= ml. of standard acid used.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">B= ml. of standard NaOH used. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Na = Normality of standard acid.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Nb = Normality of standard NaOH.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">W= Weight of the sample taken in grams.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference- Methods of Analysis, AOAC, 1965)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(v) Total nitrogen (for nitrate containing samples)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Note applicable to samples containing high concentrations of nitrate nitrogen and chlorides) </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Place weighed sample (0.7-2.2 gm) in digestion flask. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Add 40ml. H2SO4 containing 2 grams salicylic acid. Shake until thoroughly mixed and let stand, with occasional shaking, 30 minutes or more.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Then add (i) 5 grams Na2S2O3.5H2O or (ii) 2grams zinc dust (as impalpable powder not granulated zinc or filings)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Shake the flask and let it stand for five minutes. then heat over low flame until forthing ceases. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Turn off heat, add 0.7 grams copper sulphate.15 gm. powdered K2SO4) and boil briskly until solution clears, then at least 30 minutes longer (2 hours for samples containing organic material).</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Proceed further as in 6-11 of 3 (iv)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Same as in 3 (iv)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference- Methods of Analysis, AOAC, 1965).</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(vi) Total nitrogen (for materials with high Cl: NO3 ration and to materials containing only water soluble nitrogen).</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Reduced iron powder electrically reduced N.F. (National Formulary).</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">For other reagents see 3 (ii)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Mixed fertilizers</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Place 0.5-2.0 gm. sample in Kjeldahl flask and add 2-5 grams reduced Fe(5gms. is enough for 0.185 grams. NO<sub>3</sub>).</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Add approximately 25ml. distilled water, rotating flask at angle to wash down the sample. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Let it stand for 15 minutes with occasional agitation, to insure complete solution of all soluble salts.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) While rotating flask add 25ml. cold H<sub>2</sub>SO<sub>4</sub> (1+1) and let it stand until visible reaction ceases, (use hood or vented digestion unit)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Add boiling chips and boil 15-20 minutes, but do not take to dryness (For samples containing organic matter use 50ml. cold H2SO4 (1+1) boil for 15-20 minutes add 0.7 gm. MgO and heat again for 40 minutes) Cool and proceed further as in 6-11 of 3 (iv).</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Same as in 3 (iv)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference-methods of Analysis, AOAC 1965).</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(vii) Determination of ammoniacal nitrogen (Distillation Method) (This method is for the determination if nitrogen present or available in the sample as ammonium ion. This method assumes that Urea is absent from the sample. Not applicable to MgNH<sub>4</sub> PO<sub>4</sub> and Fe<sub>4</sub>PO<sub>4</sub>)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Place 0.7-3.5 grams according to HN3 content of the sample in distillation flask with approximately 300 ml. water and 2 grams of freshly ignited carbonate free MgO or NaOH </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Connect the flask to condenser by Kjeldahl connecting bulb.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Distill 100 ml. liquid into measured quantity of standard acid and titrate with standard NaOH solution, using methyl red as an indicator </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Percent nitrogen = (ANa -BNb) x 0.01401 x 100 / W&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A= ml. of standard acid used.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">B= ml. of standard NaOH.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Na = normality of acid. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Nb = normality of NaOH.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">W= weight of the sample taken in gm. </font> </span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference -Recommended analytical methods of the </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">National Plant Food Institute, Washington. D.C. 1961)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(viii) Determination of ammoniacal and nitrate nitrogen (Devarda Method)(This method is for the determination of total nitrogen when only nitrate or mixture of nitrate and ammoniacal nitrogen is present. This method assumes the absence of urea, calcium Cyanamid and organic matter from the sample.)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Place 0.35-0.5 gms. sample in600-700ml. flask and add 300ml. water, 3 grams devarda Alloy, and 5ml. NaOH solution (42 percent by weight pouring later down side of flask so that it does not mix at once with contents)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Allow the flask to stand for 15 minutes.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) By means of Davison [ J. Ind. Eng. Chem. 11,465 (1919)] or other suitable scrubbing bulb, that will prevent passing over of any spray, connect with condenser tip of which always extends beneath surface of standard acid in receiving flask. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Mix contents of distilling flask by rotating. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Heat slowly at first and then at a rate to yield 250 ml. distillate in 1 hour.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Collect distillate in measured quantity of standard acid and titrate with standard NaOH solution using methyl red as an indicator.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) In analysis of nitrate salts dissolve 3.5 or 5.0 grams in water, to 250 ml. and use 25ml. aliquot. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculation </font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Same as in 3 (iv)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(reference- Methods of Analysis, AOAC, 1965)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ix) Determination of nitrate nitrogen</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Applicable in presence of calcium Cyanamid and urea in the mixture)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Procedure </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Determine total nitrogen as in 3(v)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Determine water insoluble N as in 3(x) but use 2.5 grams sample. Dilute to 250ml. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Determine ammoniacal N in 50ml filtrate as in (vii).</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Place another 50ml. portion filtrate in 500 ml. Kjeldahl flask and 2 grams FeSO<sub>4</sub>.7H<sub>2</sub>O and 20ml. H<sub>2</sub>SO<sub>4</sub> (if total N is 5percent use 5gm. Fe SO<sub>4</sub>.7H<sub>2</sub>O) Digest over hot flame until all water is evaporated and white fumes appear and continue digestion at least ten minutes to drive off nitrate N. If severe bumping occurs add 10-15 glass beads. Add 0.65 grams Hg or 0.7 grams HgO and digest until all organic matter is oxidized, cool, dilute add the K2S solution and complete determination as 3 (iv) Before distillation add pinch of mixture of zinc dust and granular &quot;20 mesh&quot;. zinc to each flask to prevent bumping.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Total N (a)-- water insoluble N(b)- water soluble N. Water Sol. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">N-- N obtained in (d)- nitrate N. </font></span> </p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference -Methods of analysis, AOAC, 1965)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(x) Determination of water insoluble nitrogen</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Procedure </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Place 1 or 1.4 grams sample in 50ml. beaker, wet with alcohol.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Add 20ml. water and let it stand for 15 minutes stirring occasionally.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Transfer supernatant liquid to 11 cm. Whatman No. 42. paper in 60 long stem funnel 2.5&quot; diameter and wash residue 4 or 5 times by decanting with water at room temperature (20-25C)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Finally transfer all residue to filter and complete washing until filtrate measures 250ml. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Determine N as in 3(iv)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(xi) Determination of urea nitrogen</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(This method is for the determination of urea content of any mixed fertilizers.)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Neutral urease solution - shake 1gm. jack bone meal with 100ml. water for 5 minutes. Transfer 10ml solution to 250 ml. Erlenmeyer flask, dilute with 50ml. water and add 4 drops methyl purple indicator. Tiltrate with 0.1 N NaOH. From difference in ml. calculate amount of 0.1 N HCL require to neutralize remainder of solution (usually approximately 2.5 ml. per 100ml.) add this amount of acid </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Procedure </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Weight 10+0.01 gm. sample and transfer to 15cm. Whatman No. 12 fluted filter paper. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Leach with approximately 300ml. water into 500ml. volumetric flask.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Add 75-100 ml. saturated barium hydroxide solution to precipitate phosphates </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Let it settle and test for complete precipitation with few drops of saturated barium hydroxide solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Add 20ml 10 percent sodium carbonate solution to precipitate excess barium and any soluble calcium salts. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Let it settle and test for complete precipitation. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) Dilute to volume, mix and filter through 15cm. Whatman. No. 12 fluted paper.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Transfer 50ml. aliquot (equivalent to 1gm. sample)to 200 or 250 ml. Erlenmeyer flask and add 1 to 2 drops methyl 1 purple indicator.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(9) Acidify solution with 2N HCl and add 2 to 3 dorps excess. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(10) Neutralize solution with 0.1 N NaOH to first change in colour indicator. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(11) Add 20ml. neutral urease solution, close flask with rubber stopper and let it stand for 1 hour at 20-25C. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(12) Cool the flask in ice water slurry and titrate at once with 0.1 N HCl to full purple colour, then add approximately 5ml. excess.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(13) Record total volume added, back titrate excess HCl with 0.1N NaOH to neutral end point.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Percentage urea =(ml. 0.1 N HCl - ml 0.1 N NaOH) x0.3003 wt. of sample. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference- methods of Analysis, AOAC, 1965)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(xii) Determination of biuret</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Alkaline tartarate solution-- Dissolve 40gm NaOH in 50ml. water cool, add 50gm. of NaK C<sub>4</sub>H<sub>4</sub>O<sub>6</sub>4HP<sub>2</sub>Oand dilute to 1 liter. Let. it stand for one day before use. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Copper Sulphate solution - Dissolve 15 gm. CuSO<sub>4</sub>.5H<sub>2</sub>O in CO<sub>2</sub>P free water and dilute to 1 liter.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Biuret standard solution- 1mg./ml. Dissolve 100gm. reagent grade biuret in CO<sub>2</sub>free water and dilute to 100ml. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Ion exchange resin. Fill 50ml. burette with 30cm. column of Amberlite IR 120 (H) resin on glass wool plug.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Regenerate column after each use by passing 100ml. H<sub>2</sub>SO<sub>4</sub> (1+9) or HCL (1+4) through the column approximately 5ml.per minute and then washing with water until pH of effluent is 6.0.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Preparation of standard curve.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Transfer series of aliquotes, 2-50 ml. of standard biuret solution to 100ml. volumetric flask.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Adjust volume to approximately 50ml with CO<sub>2</sub> free water. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Add one drop of methyl red and neutralize with 0.1 NH<sub>2</sub>SO<sub>4</sub> to pink colour. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Add with swirling 20ml alkaline tartarate solution and then 20ml. CuSO<sub>4</sub> solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Dilute to volume. Shake for 10 seconds and place in water bath for 15 minutes at 30+5C..</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Also prepare reagent blank.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Determine absorbance of each solution against blank at 555 mw (instrument with 500-570 mw filter is also satisfactory ) with 2-4cm. cell. and plot standard curve.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp; A. In urea</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Stir continuously 2-5 gm sample in 100ml. approximately 50</font><sup><font size="2">C </font></sup> </span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">water for 30 minutes. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Filter and wash into 250 ml. volumetric flask and dilute to volume </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Transfer 25ml. aliquot to 100ml. volumetric flask and proceed as given under preparation of standard curve 3 (xii).</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">B. In mixed fertilizers.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Stir continuously 10-20gm. sample in 150 ml. approximately (50<sup> C</sup>) hot water for 30 minutes. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Filter and wash into 250ml volumetric flask and dilute to volume.</font></span><span style="font-family: Verdana; background-color: #EFEFEF"><font size="2"> </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Transfer 25 ml aliquot to column 3 (xii) (a) (4) and adjust flow to 4- 5 ml./minute. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Receive elute in 100ml. beaker. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) When liquid level falls to top of resin bed. wash with two 25ml portion water. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) To eluate and washings add two drops of methyl red and then 0.1 N NaOH to yellow colour. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) Add 0.1 NH<sub>2</sub> SO<sub>4</sub> until solution just turns pink .</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Transfer to 100ml. volumetric flask and dilute to volume with CO<sub>2</sub> free water.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(9) Transfer 50ml. aliquot to 100ml. volumetric flask and proceed as in preparation of standard curve given above. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculation</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">From standard curve determine concentration of biuret in final dilution. then percent of </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Biuret = C x 100 / W</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Where C= concentration in mg/ml of biuret in final dilution obtained from standard curve. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">W= Concentration of original sample in final dilution expressed as mg/ml.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference -Methods of analysis, AOAC, 1965)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(xiii) Determination of free acidity in ammonium sulphate (as H<sub>2</sub>SO<sub>4</sub>)</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Standard sodium hydroxide solution- 0.02 N.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Methyl red indicator--Dissolve 0.15 gm. of water soluble methyl red in 500 ml. water.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Methyl red-- Methyl blue mixed indicator solution- prepared by mixing equal volumes of 0.2 percent solution in rectified spirit of methyl red and 0.1 percent solution in rectified spirit of methylene blue.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Dissolve about 20mg. of prepared sample, accurately weighed in about 50ml. cold natural water.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Filter and make up the volume to about 200ml. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Titrate with standard sodium hydroxide solution, using one or two drops of methyl red as indicator.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) If satisfactory end point with methyl red is not obtained, methylene red-- methylene blue mixed indicator may be used. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Use- preferably a micro biuret for this titration. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">The filtering medium shall be neutral and shall not contain any alkaline material which would neutralize free acid. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Free acidity as H<sub>2</sub>SO<sub>4</sub> percent by weight =4.904AN /W</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A= Volume of ml. of standard NaOH solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">N= Normality of standard NaOH Solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">W= Weight in gm of prepared sample taken for the test.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference - Specification of ammonium sulphate, fertilizer grade IS:826- 1967)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(xiv) Determination of arsenic in ammonium sulphate (A<sub>2</sub>O<sub>3</sub>)</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Lead acetate solution- prepare 10percent solution of lead acetate with sufficient acetic acid added to clear the solution</font></span><span style="font-family: Verdana; background-color: #EFEFEF"><font size="2"> </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Dry lead acetate paper-Cut filter paper (Whatman No.1 or equivalent) into strips 70x50 mm and keep them permanently suspended in lead acetate solution in a glass stopped bottle, Before use, take out the strips and cry them in an atmosphere free from hydrogen sulphide.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Mercuric bromide solution-- Dissolve 5gm of mercuric bromide in 100ml rectified spirit.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Sensitized mercuric bromide paper strips-- cut filter paper (Whatman NO. 1 or equivalent) into strips 120x2.5 mm. Keep the strips permanently suspended in dark in a glass stoppered cylinder or amber bottle having mercuric bromide solution. Before use take out a strip, press it between sheets of filter paper and dry it in an atmosphere free from hydrogen sulphide. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Dilute sulphuric acid- approximately 5N.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Concentrated hydrochloric acid.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) Potassium iodide solution-15 percent.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Stannous chloride solution- Dissolve 80gm. of stannous chloride in 100ml. water containing 5ml. of concentrated hydrochloric acid and boil until clear solution is obtained. Add some metallic tin to the solution to prevent oxidation.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(9) Zinc- It is recommended that zinc rods prepared as described below should be used for routine work. however, pellets described may be used.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Preparation of zinc rods</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Take a clean and dry hard glass test tube of 10mm internal diameter and 20 cm. length.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Heat the test tube over a flame of bunsen or blow pipe burner and add slowly arsenic free granulated zinc in small portion (1 to 2 gm at a time) the next portion being added after the first one has completely melted.)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Continue heating and adding zinc until the melt is about 10cm. high. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Heat the clean melt for half an hour and then cool to room temperature. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Break the tube to obtain the rod of zinc</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Cut rod into pieces 20mm long. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) Coat the plane ends of the pieces with a paste of magnesium carbonate and gum arabic solution and dry.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Coat the pieces all over with 1.5 mm. thick layer or paraffin wax. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(9) When required for use, scrap off the wax from the place ends with a knife, protecting wax colour round the rods.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(10) Remove the paste from the plane ends by soaking in water and activate the exposed surface by dipping in a solution containing one part of stannous chloride solution and seven parts of concentrated hydrochloric acid. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Preparation of zinc pellets.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Treat zinc shots passing through IS sieve 570 (aperture 5660 microns) and retained on IS sieve 280 (aperture 2818 microns)with concentrated hydrochloric acid until the surface of zinc becomes clean and dully. Weight and keep under water, preventing contamination with dust.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(d) Standard sodium hydroxide solution-- approximately 20 percent. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(e) Standard arsenic trioxide solution </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Dissolve 1.0 gm. of resublimed arsenic trioxide (AS<sub>2 </sub>O<sub>3</sub>) in 25 ml. sodium hydroxide solution and neutralize with dilute sulphuric acid.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Dilute with freshly distilled water containing 10ml of concentrated sulphuric acid per liter and make up the volume to 1 liter. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Again dilute 10ml. of this solution to 1 liter with water containing sulphuric acid and finally dilute 100ml. of this solution to 1 liter with water containing sulphuric acid. One ml. of this solution contains 0.001 mg. of arsenic trioxide (AS2O3) the dilute solution shall be prepared freshly when required. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(f) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Dissolve 1.0 gm. of the prepared sample in 20ml water.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Place dry lead acetate paper in the lower portion of the tube B (in Figure 6) and glass wool moistened with lead acetate solution in its proper portion.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Place the sensitized strips of mercuric bromide paper in tube A and connect the tubes together with a rubber stopper.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Introduce the solution of the material into the bottle C (120 ml) and then add 10ml of dilute sulphuric acid. Add 0.5 ml. of stannous chloride solution 5ml. potassium iodide solution and make up the volume with water to about 50ml. (Figure No. 6- Modified Gutzet Method of test for arsenic.)&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Mix the contents and drop about 10mg. of zinc. Immediately fit in position the rubber stopper carrying the tube B.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Place the bottle </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) At the end of two hours remove the test strip by means of tweezers. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Carry out the test prescribed above using a volume of standard arsenic trioxide solution containing 0.1 mg. of arsenic trioxide in place of the solution of the material and compare the stain produced with the material with that produced with arsenic trioxide solution </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(9) The limit prescribed in the material specification shall be taken as not having been exceeded if the length of the stain as well as the intensity of its colour produced in the test with the material is not greater than those produced with the arsenic solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference- Modified Gutzet Method of test for arsenic , IS-2088, 1962)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(xv) Determination of calcium nitrate (for calcium ammonium nitrate and nitrophosphates.)</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) N-Amyl Alcohol.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Dilute hydrochloric acid- approximately 4N. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Standard calcium Solution-- weigh 1.0 gm of calcium carbonate dried at 120<sup>0</sup>+5<sup>0</sup>C and dissolve in the minimum quantity of dilute hydrochloric acid. Dilute the solution to 1 litre in a graduated flask. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Ammonium chloride- ammonium hydroxide buffer solution . Dissolve 67.5 gm. ammonium chloride in a mixture of 570ml. of ammonium hydroxide (sp. gr. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">0.92) and 250 ml. water. Also dissolve separately a mixture of 0.931 gm. of disodium ethylene diamine tetra-acetate dihydrate and 0.616 gm of disodium ethylene diamine tetra-acetate dihydrate and 0.616 gm of magnesium sulphate (Mg. SO<sub>4</sub>. 7H<sub>2</sub>O) in about 50ml. of water. Mix the two solutions and dilute to 1 liter.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Standard disodium ethylene diamine tetra-acetate (EDTA) solution- weight. 3.72gm. of disodium ethylene diamine tetraacetate dihydrate in water and dilute in a graduated flask to 1 liter. The solution shall be standardized frequently against standard calcium solution following the procedure given below.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Eriochrome black-T Indicator solution- Dissolve 0.1 gm in 20ml of rectified spirit. The solution shall be used for not more than a week.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Grind quickly about 5gm. of the material, accurately weighed, with about 50ml. of amyl alcohol in a pestle and mortar and transfer the contents to a conical flask. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Wash the pestle and mortar with a few ml. of amyl alcohol and add the washings to the flask.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Shake the content of the flask manually or in a mechanical shaker for about half an hour and then filter. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Transfer the filtrate to a separating funnel and extract calcium nitrate completely with water in five to six instalments. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) A few drops of dilute hydrochloric acid may be added during the extraction with water to avoid formation of an emulsion of amyl alcohol with water.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Concentrate the water extract at low temperature to nearly half its volume. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) Transfer the concentrated solution to a conical flask add 5ml. of ammonium chloride- ammonium hydroxide buffer solution, 5 drops of eriochrome black-T indicator solution and titrate against standard EDTA solution to a pure blue end point.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calcium nitrate percent by weight = 8.2 NV / W</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Where N= Normality of standard EDTA solution</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">V= Volume in ml. of standard EDTA solution used in the titration and </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">W= Weight in gm. of the material taken for test. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference--IS specifications of CAN IS: 2409-1963)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(xvi) Determination of chlorides other than ammonium chloride</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Standard silver nitrate solution- 0.1N.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Concentrated nitric acid- conforming to IS:264-1950</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Ferrous ammonium sulphate solution saturated in water and stabilized by addition of 50ml nitric acid. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Standard ammonium thiocyanate solution - 0.1 N. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Dissolve about 0.2 gm. of the prepared sample, previously dried as in procedure for determination of moisture and accurately weighted in about 40ml water. &nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Add exactly 50ml. of standard silver nitrate solution and 5ml. of concentrated nitric acid. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Add 0.5 ml. of nitrobenzence and make up the volume of the mixture to exactly 100ml. with water. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Take exactly 50ml.. of the solution and add 2ml. of ferric ammonium sulphate solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Titrate the excesses of silver nitrate in this portion with standard ammonium thiocyanate solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Carry out a blank test following the procedure given as above but without using the material. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Calculations</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Total chlorides (as Cl) percent = 7.07 (V<sub>1</sub>- V<sub>2</sub>)N</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">by weight (on dry basis) W</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Where </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">V<sub>1</sub>= Volume in ml. of standard ammonium thiocyanate used in the blank determination. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">V<sub>2</sub>= Volume in ml. of standard ammonium thiocyanate </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">solution used in the test with the material.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">N= Normality of standard ammonium thiocyanate solution.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">W= Weight in gm. of the drived prepared sample taken forthe test.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Express the ammoniacal nitrogen content percent by weight of the material determined earlier in terms of Cl as follows.Chloride equivalent of the ammoniacal nitrogen content percent by weight = 2.531 x A .....Y where A is the ammoniacal nitrogen content determined earlier. Balanced chloride equivalent to sodium chloride </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(NaCl) percent by weight=1 - 648 x (X-Y)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(x-y) = Balanced chlorides other than ammonium chloride </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference- IS Specification for ammonium chloride Fertilizers grade (Revised) IS: 1114 -1964 calculations modified.)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <b><font color="#882E0F"><span style="font-family: Verdana; background: #EFEFEF"> <font size="2">4. Determination of phosphates.</font></span></font></b></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Methods of determination of total phosphates, water soluble phosphates, citrate soluble phosphates, citrate insoluble phosphates and citric acid soluble phosphates have been described separately in this section. These methods are applicable to straight as well as mixed phosphatic fertilizers.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(i) Preparation of solution of the samples.(Separate methods of preparing solutions of the samples have been described according to the nature of the sample.)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagent</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Magnesium nitrate solution- Dissolve 950mg.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">P-free Mg(NO3)2 6H2 in water and dilute to 1litre.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Treat 1gm sample by (A),(B),(C),(D) or (E) method depending on the nature of the sample.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Cool solution transfer to 200 to 250ml. volumetric flask dilute to volume, mix and filter through dry filter. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(A) (Suitable for materials containing small quantities of organic matter) Dissolve in 30ml. HNO<sub>3</sub> and 3-5 ml. HCl and boil until organic matter is destroyed. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(B) (Suitable for fertilizers containing much Fe or Al phosphate and basic slag). Dissolve in 15-30 ml. HCl and 3-10 ml. HNO<sub>3</sub>.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(C) (Suitable for organic material like cotton seed meal alone or in mixture). Evaporate with 5ml. Of the Mg. (NO<sub>3</sub>)<sub>2</sub> solution, ignite and dissolve in HCl.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(D) (Generally applicable to materials or mixtures containing large quantities of organic matter). Boil with 20-30 ml. H<sub>2</sub>SO<sub>4</sub> in 200ml.flask adding 2-4 gm of NaNO<sub>3</sub> or KNO<sub>3</sub>at beginning of digestion and small quantity after solution is nearly colourless, or adding the nitrate in small portions from time to time. When solution is colourless, cool, add 150 ml. Water and boil for few minutes. Before adding NaNO<sub>3</sub> or KNO<sub>3</sub> let mixture digest, at gentle heat if necessary, until violence of reaction is over. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(E) (Suitable for all fertilizers). Boil gently for 30-45 minutes with 20-30ml. HNO3 in a suitable flask (preferably a Kjeldahl for samples containing large quantities of organic matter to oxidize all easily oxidizable matter) Cool and add 10-20 ml. of 70-72 percent nearly so and white dense fumes appear in flask. Do not boil to dryness at any time (danger). (with samples containing large quantities of organic matter temperature should be raised to fuming point approximately 170<sup>C </sup>over a period of 1 hour at least) Cool slightly, add 50ml. water and boil for few minutes.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(ii) Gravimetric quinoline, molybdate method for determination of total phosphorus.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Citric molybdic acid reagent- Dissolve 54 gm. 100 percent molybdic anhydride (MoO<sub>3</sub>) and 12gm. NaOH with stirring in 400ml. hot water and cool. Dissolve 60gm. citric acid in mixture of 140 ml. HCL and 300ml. water and cool. Gradually add molybdic solution to citric acid solution with stirring. Cool, filter and dilute to 1litre. (Solution may be green or blue colour depends on exposure to light). If necessary add 0.5 percent KrO<sub>3</sub> solution drop by drop until green colour becomes pale. Store in dark in polyethylene bottle </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Quinoline solution -Dissolve 50ml. synthetic quinoline with stirring in mixture of 60ml. HCl and 300ml Water. Cooldilute to 1 litre, and filter. Store in polyethylene bottle.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Quimociac reagent- Dissolve 70gm. of sodium molybdate dihydrate in 150 ml. water Dissolve 60gm citric acid in mixture of 85ml. HNO<sub>3</sub> and 150ml. water and cool. Gradually add molybdate solution to citric acid-nitric acid mixture with stirring. Dissolve 5ml. synthetic quionoline in mixture of 35nl. HNO<sub>3</sub> and 100ml. water Gradually add this solution to molybdate citric -nitric acid. solution mix and let it stand for 24 hours. Filter add 28 ml. acetone. dilute to 1 litre with water and mix well. Store in polyethylene bottle.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Treat 1mg. sample as prescribed in 4(1) and dilute it to 200ml.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Pipette into 500ml erlenmeyer flask aliquot containing not more than 25mg. P2O5 dilute to approximately 100ml with water. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Proceed with one of the following methods.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A. Add 30ml. citric molybdic acid reagent and boil gently for 3 minutes. (Solution must be precipitate free at this stage) Remove from heat and swirl carefully. Immediately add from burette 10ml quinoline solution with continuous swirling (Add first 3-4 ml drop wise and remainder in steady steam) or</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">B. Add 50ml quimociac reagent, cover with watch glass place on hot plate in well ventilated hood and boil for 1 minute. After treatment with A or B cool to room temperature, swirl carefully 3-4 times during cooling filter into gooch with glass fibre filter paper previously dried at 250 C and weighed, and wash five times with 25ml. portion of water. Dry cruicible andcontents for 30 minutes at 250C. cool in desiccator to constantweight as (C9H7N)<sub> 3</sub>H<sub>3</sub>PO<sub>4</sub>.12 MoO<sub>3</sub> subtract weight reagent blank.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Multiply by 0.03207 to obtain weight of P<sub>2</sub>O<sub>5</sub>. Report as percent P<sub>2</sub>O<sub>5</sub>.</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iii) Determination of water soluble phosphorus</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Place 1gm sample on 9cm filter paper and wash with small portion of water until filtrate measure approximately 259ml. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Let each portion pass through filter before adding more and use suction if washing would not otherwise be complete within 1 hour. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) If the filtrate is turbid, add 1-2 ml. HNO<sub>3</sub>dilute to 250ml and mix. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Pipette into 500ml. Erlenmeyer flask aliquot containing not more than 25mg. P<sub>2</sub>O<sub>5</sub>. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Dilute if necessary to 50ml.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Add 10ml. HNO<sub>3</sub> (1plus 1) and boil gently for 10minutes. Cool and dilute to 100ml. and proceed as 4(ii) (b)(2) (B).</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(reference- methods of analysis AOAC, 1965)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(iv) Citrate insoluble phosphorus </font></span> </p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents </font></span></p> <ol style="margin-top: 0in; margin-bottom: 0in" start="1" type="1"> <li class="MsoNormal" style="text-align: justify"> <p style="margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Ammonium citrate solution - should have specific gravidity of 1.09 at 20<sup>0</sup>C and pH of 7.0 as determined electometrically. </font></span></li> </ol> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Dissolve 370 gm crystalline citric acid in 1.5 litre distilled water and nearly neutralize by adding 345 ml. NH<sub>4</sub>OH (28-29% NH3) if concentration of ammonia is less than 28 percent add correspondingly larger volume, and dissolve citric acid in correspondingly smaller volume of water, cool and check pH. Adjust with NH<sub>4</sub> OH (1 plus 7) or citric acid solution to pH 7.Dilute solution if necessary to specific gravity of 1.09 at 20<sup>0 </sup>C(Volume will be approximately 2 litres) Keep in tightly stoppered bottles and check pH from time to time. If pH has changed from 7.0 readjust. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <ol style="margin-top: 0in; margin-bottom: 0in" start="2" type="1"> <li class="MsoNormal" style="text-align: justify"> <p style="margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Other reagents and solutions as in 4(i) and 4(ii)</font></span></li> </ol> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Procedure (acidulated samples and mixed fertilizers)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) After removing water soluble P<sub>2</sub>O<sub>5</sub>. in 4(iii) transfer filter and residue within 1 hour to 200or 250 ml flask containing 100ml. ammonium acetate solution previously heated to 65<sup>0</sup>C.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Close flask tightly with smooth rubber stopper.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Shake vigorously until paper is reduced to pulp and relieve pressure by removing stopper momentarily. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) continuously agitate contents of stopper flask in apparatus equiped to hold contents of flask at exactly 65<sup>0</sup>C. (Action of apparatus should be such that dispersion of sample in citrate solution is continually maintained and entire inner surface of flask and stopper is continually bathed with solution). </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Exactly 1 hour after adding filter and residue, remove flask from apparatus and immediately filter contents by suction as rapidly as possible through Whatman No. 5 paper or equivalent. using buchner or ordinary funnel with platinum or other cone. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Wash with distilled water and at 65<sup>0</sup>C until volume of filtrate is approximately 350ml. allowing time for through draining before adding more water.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) If material is one that will yield cloudy filtrate wash with 2 percent NH<sub>4 </sub>NO<sub>3</sub> solution. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Determine P<sub>2</sub>O<sub>5</sub>. in citrate insoluble residue by one of the following methods. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A. Dry paper and contents transfer to crucible ignite until all organic matter is destroyed and digest with 10-15 ml. HCl until all phosphate dissolve or.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">B. Treat wet filter and contents a s in method prescribed in 4(i) (b) (2) (A) (C) (D) or (E) Dilute solution to 250ml. or other suitable volume, mix well filter through dry paper and determine P<sub>2</sub>O<sub>5</sub>. as in 4 (ii)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference - methods of Analysis, AOAC, 1965)</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(v) Citrate soluble phosphorus</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(Reference S.O. 403 (E) dated 23 May, 1990)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">Subtract citrate insoluble P<sub>2</sub>O<sub>5</sub>. from total P<sub>2</sub>O<sub>5</sub>.to obtain citrate soluble P<sub>2</sub>O<sub>5</sub>. in fertilizers other than basic slag.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(a) Reagents</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Concentrated hydrochloric acid.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Concentrated citric acid.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Calcium carbonate finely ground</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) 5 N Sodium hydroxide solution. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Dilute hydrochloric acid- Dilute 240 ml or concentrated hydrochloric acid with water to 1 litre</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp; (6) Citric molybdic acid solution- Stir 54 gm of molybdic anhydride (MoO<sub>3</sub>) with 200ml. of water add 11gm of sodium hydroxide and stir the mixture whilst heating to boiling point until the molybdic whilst heating to boiling point until the molybdic anhydride dissolves. Dissolve 60gm of citric acid in about 250to 300 ml of water and add 140 ml of concentrated hydrochloric acid. Pour the molybdate solution into the acid solution. Which is stirred solution through paper pulp pad. Dilute the solution to 1 litre. If the solution is slightly green or blue in colour add dropwise a dilute (0.5 to 1.0 percent) solution of potassium bromate until the colour is discharged. This reagent should be kept in dark.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) Quinoline solution- Measure 60ml of concentrated hydrochloric acid and 300 to 400 ml of water into 1 litre beaker and warm to 70<sup>0</sup>C-80<sup>0</sup>C pour 50ml. of quinoline in a thin stream into the dilute acid while stirring. When quinoline has dissolved. cool the solution dilute acid to 1 litre and if necessary filter through a paper pulp filter.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Sodium hydroxide solution- 0.5 N carbonate free.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(9) Indicator solution- Mix three volumes of thymol blue solution and two volumes of phenolphthalein solution prepared as follows </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">A. Thymol blue solution- Dissolve 250mg. thymol blue in 5.5 ml of 0.1 N sodium hydroxide solution and 125 ml of industrial methylated spirit. Dilute with water to 250ml. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">B. Phenolphthalein solution- Dissolve 250mg. phenolphthalein in 150 ml of industrial methylated spirit and dilute with water to 250ml.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(10) Hydrochloric acid- 0.5N.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(11) Sodium hydroxide solution- 0.1N.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(12) Hydrochloric acid- 0.1 N.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(13) Surface active agent- 0.5 percent solution of sodium dodecyi benzene sulphonate suitable. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background-color: #EFEFEF"> <font size="2">&nbsp;</font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(b) Preparation of solution</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Weigh to the nearest mg. about 5gm. of the sample and transfer to a stoppered bottle of about 1 litre capacity.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Dissolve 10gm. of pure crystallized citric acid (monohydrate) in water dilute to 500ml and adjust the temperature to 20<sup>0</sup>C</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) Add the solution to the sample in the bottle, shaking so as to avoid the possibility of caking. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Shake the bottle continuously for 30 minutes. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Pour whole of the liquid at once on to a large medium fine filter. and collect the filtrate. If the filtrate is not clear, pass it again through the same filter. </font></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana"> <span style="background-color: #EFEFEF"><font size="2">&nbsp;</font></span><span style="background: #EFEFEF"><font size="2">&nbsp;</font></span></span></p> <p class="MsoNormal" style="text-align: justify; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(c) Procedure</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(1) Transfer a volume of the solution prepared according to procedure given above containing less than 70mg. of phosphoric acid and preferably about 50mg. to a 500ml stoppered conical flask marked at 150ml. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(2) Dilute the solution with water to 100ml. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(3) If the sample does not contain calcium add 100 to 200mg. of calcium carbonate. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(4) Then add 5 N sodium hydroxide solution dropwise until a faint permanent turbidity or precipitate is formed. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(5) Dissolve the precipitate by the dropwise addition of dilute hydrochloric acid but avoid an excess.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(6) Dilute to 150 ml and add 50ml of the citric-molybdic acid reagent and heat the solution to incipient ebullition, maintain it at this temperature for 3 minutes and then bring it to the boiling point. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(7) From burette slowly add 25ml of the quinoline solution with constant swirling throughout the first few ml. being added dropwise, the rest in slow stream. </font></span> </p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(8) Keep the solution gently boiling during the addition.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(9) Immerse the flask in boiling water for 5 minutes, then cool it to 15<sup>0</sup>C in funning water.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(10) Filter with suction the contents of the flask on a paper pulp pad, and wash the flask precipitate and filter with successive small washes of cold water until they are free from acid. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(11) Transfer the filter pad and precipitate to the original flask, rinse the funnel with water and collect the rinsings in the flask. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(12) If necessary, wipe the funnel with small piece of damp filter paper to ensure complete removal of the precipitate and place the paper in the flask. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(13) Add water to a total of about but not exceeding 100ml Stopper the flask and shake it vigorously until the pulp and precipitate are completely dispersed. </font> </span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(14) Remove the stopper and wash it with water returning the washing of the flask. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(15) Add a measured volume of 0.5 N sodium hydroxide solution sufficient to dissolve the precipitate and leave a few ml. in excess.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(16) Shake the flask vigorously until all the precipitate dissolves. (To facilitate the dispersal of the precipitate, after the addition of 0.5 N sodium hydroxide solution a few drops of the surface active agent may be added if necessary)</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(17) Add 0.5 -1.0 ml of the indicate solution and titrate the excess of sodium hydroxide with 0.5 N hydrochloric acid until the indicator changes from violet to green-blue and then very sharply to yellow at the end point. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(18) Deduct the number of ml of 0.5 N hydrochloric acid used from the number of ml. 0.5 N sodium hydroxide equivalent to the phosphoric acid.</font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(19) Carry out a blank determination on all the reagents. omitting only the sample and using 0.1 N standard alkali and acid instead of 0.5 N for the titration. Calculate the blank in terms of 0.5 N alkali and subtract it from the original result. </font></span></p> <p class="MsoNormal" style="text-align: justify; text-indent: .5in; margin-top: 0; margin-bottom: 0"> <span style="font-family: Verdana; background: #EFEFEF"> <font size="2">(20) Calculate the amount of phosphoric acid in the por