CIPAC Meeting 2027
Xi'An, China
CIPAC Meeting 2027

MT 110 - Mercurial impurities in technical and formulated mercurials


Content Handbook F

 

Outline of method

110.1 General TLC method for samples containing more than 1% of inorganic mercury

The sample is dissolved in acetone/aqueous sodium chloride or dioxane/aqueous sodium chloride. The solution is spotted on to a silica gel TLC plate, developed with carbon tetrachloride/acetone, and sprayed with copper(II) sulphate and potassium iodide/sodium sulphite solutions. The resulting spots are compared with standard spots from pure mercury(II) chloride to give the inorganic mercury content of the sample.

110.2 Gravimetric method

Inorganic and any organic mercury compounds soluble in acetic acid are extracted from the sample by stirring it with hot acetic acid. The mixture is filtered, the filtrate is neutralized with ammonia, and potassium iodide is added to precipitate phenylmercury(II) compound as phenylmercury(II) iodide which is filtered off. The filtrate is heated with bis(ethylenediamine) copper(II) sulphate solution to form an insoluble mercury complex [bis(ethylenediamine)mercury(II) sulphate] which is then filtered off, and weighed.

110.3 Sulphide colorimetric method

110.3.1 Ethylmercury(II) chloride and phenylmercury(II) chloride -Determination of inorganic mercury salts.

The sample is dissolved in acetone and the solution is saturated with hydrogen sulphide. The colour of the solution is compared with standards prepared in a similar manner from mercury(II) chloride.

110.3.2 Mercury(II) iodide - Determination of water-soluble mercury(II)compounds

The sample is shaken with water, filtered and the filtrate is treated with hydrogen sulphide. The colour of the solution is compared with standards prepared in a similar manner from mercury(II) chloride.

110.3.3 Mercury(II) oxide technical - Determination of other mercury salts

The sample is shaken with dilute ethanol, filtered and the filtrate is treated with hydrogen sulphide. The colour of the solution is compared with standards prepared in a similar manner from mercury(II) chloride.

110.3.4 Mercury(I) oxide technical - Determination of mercury(II) chloride

The mercury(II) chloride is extracted with diethyl ether, the ether is evaporated off and the residue dissolved in water. The solution is treated with hydrogen sulphide. The colour of the solution is compared with standards prepared in a similar manner from mercury(II) chloride.

110.3.5 Phenylmercury(II) dimethyldithiocarbamate - Determination of inorganic mercury(II) salts.

The sample is shaken with acetone, filtered, and the filtrate is treated with hydrogen sulphide. The colour of the solution is compared with standards prepared in a similar manner from mercury(II) chloride.

110.4 2-Ethoxyethylmercury(II) and 2-methoxyethyl(II) chlorides

The sample is dissolved in sodium hydrogencarbonate solution, any insoluble material is filtered off and its mercury content determined by oxidation with sulphuric acid and potassium nitrate.

110.5 Mercurial seed treatments containing mercury(II) chloride and/or iodide - Determination of free mercury and mercury from mercury(I) salts

The sample is extracted with hot methanol and filtered. Any soluble material is refluxed with zinc and acetic acid. The resultant zinc amalgam is dissolved in nitric acid and the mercury content is determined by titration with standard thiocyanate solution.

110.6 Phenyl mercury(II) chloride - Determination of water-soluble inorganic and/or organic mercury compounds

The material is shaken with water, filtered and the filtrate is treated with hydrogen sulphide.
If the solution blackens, then water-soluble mercury(II) salts are present. Reject the sample. If any white precipitate is produced, filter off, digest in the normal manner and determine the content of soluble organic mercury.

 

Scope

110.1 General TLC method for samples containing more than 1% of inorganic mercury

The method is suitable for the determination of 1 to 14% inorganic mercury salts in technical and formulated organomercury(II) compounds.

110.2 Gravimetric method

The method is suitable for the determination of inorganic mercury, in phenylmercury(II) acetate, chloride and nitrate.

 


Failed to start the session because headers have already been sent by "D:\www\www83\plugins\system\debug\src\Extension\Debug.php" at line 377. (500 Whoops, looks like something went wrong.)

RuntimeException RuntimeException

HTTP 500 Whoops, looks like something went wrong.

Failed to start the session because headers have already been sent by "D:\www\www83\plugins\system\debug\src\Extension\Debug.php" at line 377.

Exceptions 2

RuntimeException

in D:\www\www83\libraries\vendor\joomla\session\src\Storage\NativeStorage.php (line 454)
  1. if ($this->isActive()) {
  2. throw new \RuntimeException('Failed to start the session: already started by PHP.');
  3. }
  5. if (ini_get('session.use_cookies') && headers_sent($file, $line)) {
  6. throw new \RuntimeException(
  7. sprintf('Failed to start the session because headers have already been sent by "%s" at line %d.', $file, $line)
  8. );
  9. }
  11. if (!session_start()) {
NativeStorage->start() in D:\www\www83\libraries\src\Session\Storage\JoomlaStorage.php (line 313)
  1. $this->setId($session_clean);
  2. $cookie->set($session_name, '', ['expires' => time() - 3600 ]);
  3. }
  4. }
  6. parent::start();
  8. // Try loading data from the session
  9. if (!empty($_SESSION['joomla'])) {
  10. $this->data = unserialize(base64_decode($_SESSION['joomla']));
  11. }
JoomlaStorage->start() in D:\www\www83\libraries\vendor\joomla\session\src\Session.php (line 396)
  1. {
  2. if ($this->isStarted()) {
  3. return;
  4. }
  6. $this->store->start();
  8. $this->setState(SessionState::ACTIVE);
  10. // Initialise the session
  11. $this->setCounter();
Session->start() in D:\www\www83\libraries\vendor\joomla\session\src\Session.php (line 327)
  1. * @since 1.0
  2. */
  3. public function has($name)
  4. {
  5. if (!$this->isActive()) {
  6. $this->start();
  7. }
  9. return $this->store->has($name);
  10. }
Session->has() in D:\www\www83\libraries\src\Session\Session.php (line 194)
  2. $name = $args[2] . '.' . $name;
  3. }
  4. }
  6. if (parent::has($name)) {
  7. // Parent is used because of b/c, can be changed in Joomla 6
  8. return parent::get($name, $default);
  9. }
  11. /*
Session->get() in D:\www\www83\libraries\src\Factory.php (line 372)
  1. __CLASS__
  2. ),
  3. E_USER_DEPRECATED
  4. );
  6. $instance = self::getApplication()->getSession()->get('user');
  8. if (\is_null($id)) {
  9. if (!($instance instanceof User)) {
  10. $instance = User::getInstance();
  11. }
Factory::getUser() in D:\www\www83\libraries\src\Document\Renderer\Html\ModulesRenderer.php (line 46)
  1. {
  2. $renderer = $this->_doc->loadRenderer('module');
  3. $buffer = '';
  5. $app = Factory::getApplication();
  6. $user = Factory::getUser();
  7. $frontediting = ($app->isClient('site') && $app->get('frontediting', 1) && !$user->guest);
  8. $menusEditing = ($app->get('frontediting', 1) == 2) && $user->authorise('core.edit', 'com_menus');
  10. foreach (ModuleHelper::getModules($position) as $mod) {
  11. $moduleHtml = $renderer->render($mod, $params, $content);
ModulesRenderer->render() in D:\www\www83\libraries\src\Document\HtmlDocument.php (line 578)
  2. $cbuffer[$hash] = $tmpdata;
  4. $cache->store($cbuffer, 'cbuffer_' . $type);
  5. } else {
  6. $this->setBuffer($renderer->render($name, $attribs, null), $type, $name, $title);
  7. }
  9. return parent::$_buffer[$type][$name][$title];
  10. }
HtmlDocument->getBuffer() in D:\www\www83\libraries\src\Document\HtmlDocument.php (line 897)
  1. $replace = [];
  2. $with = [];
  4. foreach ($this->_template_tags as $jdoc => $args) {
  5. $replace[] = $jdoc;
  6. $with[] = $this->getBuffer($args['type'], $args['name'], $args['attribs']);
  7. }
  9. return str_replace($replace, $with, $this->_template);
  10. }
  11. }
HtmlDocument->_renderTemplate() in D:\www\www83\libraries\src\Document\HtmlDocument.php (line 650)
  2. if (\array_key_exists('csp_nonce', $params) && $params['csp_nonce'] !== null) {
  3. $this->cspNonce = $params['csp_nonce'];
  4. }
  6. $data = $this->_renderTemplate();
  7. parent::render($caching, $params);
  9. return $data;
  10. }
HtmlDocument->render() in D:\www\www83\libraries\src\Document\ErrorDocument.php (line 139)
  1. $this->debug = $params['debug'] ?? false;
  2. $this->error = $this->_error;
  4. $params['file'] = 'error.php';
  6. return parent::render($cache, $params);
  7. }
  9. /**
  10. * Render the backtrace
  11. *
ErrorDocument->render() in D:\www\www83\libraries\src\Error\Renderer\HtmlRenderer.php (line 70)
  1. ob_end_clean();
  2. }
  4. $this->getDocument()->setTitle(Text::_('Error') . ': ' . $error->getCode());
  6. return $this->getDocument()->render(
  7. false,
  8. [
  9. 'template' => $template->template,
  10. 'directory' => JPATH_THEMES,
  11. 'debug' => JDEBUG,
HtmlRenderer->render() in D:\www\www83\libraries\src\Exception\ExceptionHandler.php (line 142)
  1. 'subject' => $app,
  2. 'document' => $renderer->getDocument(),
  3. ])
  4. );
  6. $data = $renderer->render($error);
  8. // If nothing was rendered, just use the message from the Exception
  9. if (empty($data)) {
  10. $data = $error->getMessage();
  11. }
ExceptionHandler::render() in D:\www\www83\libraries\src\Exception\ExceptionHandler.php (line 76)
  1. * @since 3.10.0
  2. */
  3. public static function handleException(\Throwable $error)
  4. {
  5. static::logException($error);
  6. static::render($error);
  7. }
  9. /**
  10. * Render the error page based on an exception.
  11. *
ExceptionHandler::handleException() in D:\www\www83\libraries\src\Application\CMSApplication.php (line 334)
  1. );
  3. // Trigger the onError event.
  4. $this->dispatchEvent('onError', $event);
  6. ExceptionHandler::handleException($event->getError());
  7. }
  9. // Trigger the onBeforeRespond event.
  10. $this->dispatchEvent(
  11. 'onBeforeRespond',
CMSApplication->execute() in D:\www\www83\index.php (line 35)
  2. // Run the application - All executable code should be triggered through this file
  3. require_once dirname(__FILE__) . '/includes/app.php';
  5. $app = JFactory::getApplication('site');
  6. $app->execute();

RuntimeException

Failed to start the session because headers have already been sent by "D:\www\www83\plugins\system\debug\src\Extension\Debug.php" at line 377.

in D:\www\www83\libraries\vendor\joomla\session\src\Storage\NativeStorage.php (line 454)
  1. if ($this->isActive()) {
  2. throw new \RuntimeException('Failed to start the session: already started by PHP.');
  3. }
  5. if (ini_get('session.use_cookies') && headers_sent($file, $line)) {
  6. throw new \RuntimeException(
  7. sprintf('Failed to start the session because headers have already been sent by "%s" at line %d.', $file, $line)
  8. );
  9. }
  11. if (!session_start()) {
NativeStorage->start() in D:\www\www83\libraries\src\Session\Storage\JoomlaStorage.php (line 313)
  1. $this->setId($session_clean);
  2. $cookie->set($session_name, '', ['expires' => time() - 3600 ]);
  3. }
  4. }
  6. parent::start();
  8. // Try loading data from the session
  9. if (!empty($_SESSION['joomla'])) {
  10. $this->data = unserialize(base64_decode($_SESSION['joomla']));
  11. }
JoomlaStorage->start() in D:\www\www83\libraries\vendor\joomla\session\src\Session.php (line 396)
  1. {
  2. if ($this->isStarted()) {
  3. return;
  4. }
  6. $this->store->start();
  8. $this->setState(SessionState::ACTIVE);
  10. // Initialise the session
  11. $this->setCounter();
Session->start() in D:\www\www83\libraries\vendor\joomla\session\src\Session.php (line 327)
  1. * @since 1.0
  2. */
  3. public function has($name)
  4. {
  5. if (!$this->isActive()) {
  6. $this->start();
  7. }
  9. return $this->store->has($name);
  10. }
Session->has() in D:\www\www83\libraries\src\Session\Session.php (line 194)
  2. $name = $args[2] . '.' . $name;
  3. }
  4. }
  6. if (parent::has($name)) {
  7. // Parent is used because of b/c, can be changed in Joomla 6
  8. return parent::get($name, $default);
  9. }
  11. /*
Session->get() in D:\www\www83\libraries\src\Factory.php (line 372)
  1. __CLASS__
  2. ),
  3. E_USER_DEPRECATED
  4. );
  6. $instance = self::getApplication()->getSession()->get('user');
  8. if (\is_null($id)) {
  9. if (!($instance instanceof User)) {
  10. $instance = User::getInstance();
  11. }
Factory::getUser() in D:\www\www83\libraries\src\Application\SiteApplication.php (line 565)
  1. *
  2. * @since 3.2
  3. */
  4. protected function initialiseApp($options = [])
  5. {
  6. $user = Factory::getUser();
  8. // If the user is a guest we populate it with the guest user group.
  9. if ($user->guest) {
  10. $guestUsergroup = ComponentHelper::getParams('com_users')->get('guest_usergroup', 1);
  11. $user->groups = [$guestUsergroup];
SiteApplication->initialiseApp() in D:\www\www83\libraries\src\Application\SiteApplication.php (line 237)
  1. * @since 3.2
  2. */
  3. protected function doExecute()
  4. {
  5. // Initialise the application
  6. $this->initialiseApp();
  8. // Mark afterInitialise in the profiler.
  9. JDEBUG ? $this->profiler->mark('afterInitialise') : null;
  11. // Route the application
SiteApplication->doExecute() in D:\www\www83\libraries\src\Application\CMSApplication.php (line 304)
  1. $this->sanityCheckSystemVariables();
  2. $this->setupLogging();
  3. $this->createExtensionNamespaceMap();
  5. // Perform application routines.
  6. $this->doExecute();
  8. // If we have an application document object, render it.
  9. if ($this->document instanceof \Joomla\CMS\Document\Document) {
  10. // Render the application output.
  11. $this->render();
CMSApplication->execute() in D:\www\www83\index.php (line 35)
  2. // Run the application - All executable code should be triggered through this file
  3. require_once dirname(__FILE__) . '/includes/app.php';
  5. $app = JFactory::getApplication('site');
  6. $app->execute();

Stack Traces 2

[2/2] RuntimeException 
RuntimeException:
Failed to start the session because headers have already been sent by "D:\www\www83\plugins\system\debug\src\Extension\Debug.php" at line 377.

  at D:\www\www83\libraries\vendor\joomla\session\src\Storage\NativeStorage.php:454
  at Joomla\Session\Storage\NativeStorage->start()
     (D:\www\www83\libraries\src\Session\Storage\JoomlaStorage.php:313)
  at Joomla\CMS\Session\Storage\JoomlaStorage->start()
     (D:\www\www83\libraries\vendor\joomla\session\src\Session.php:396)
  at Joomla\Session\Session->start()
     (D:\www\www83\libraries\vendor\joomla\session\src\Session.php:327)
  at Joomla\Session\Session->has()
     (D:\www\www83\libraries\src\Session\Session.php:194)
  at Joomla\CMS\Session\Session->get()
     (D:\www\www83\libraries\src\Factory.php:372)
  at Joomla\CMS\Factory::getUser()
     (D:\www\www83\libraries\src\Document\Renderer\Html\ModulesRenderer.php:46)
  at Joomla\CMS\Document\Renderer\Html\ModulesRenderer->render()
     (D:\www\www83\libraries\src\Document\HtmlDocument.php:578)
  at Joomla\CMS\Document\HtmlDocument->getBuffer()
     (D:\www\www83\libraries\src\Document\HtmlDocument.php:897)
  at Joomla\CMS\Document\HtmlDocument->_renderTemplate()
     (D:\www\www83\libraries\src\Document\HtmlDocument.php:650)
  at Joomla\CMS\Document\HtmlDocument->render()
     (D:\www\www83\libraries\src\Document\ErrorDocument.php:139)
  at Joomla\CMS\Document\ErrorDocument->render()
     (D:\www\www83\libraries\src\Error\Renderer\HtmlRenderer.php:70)
  at Joomla\CMS\Error\Renderer\HtmlRenderer->render()
     (D:\www\www83\libraries\src\Exception\ExceptionHandler.php:142)
  at Joomla\CMS\Exception\ExceptionHandler::render()
     (D:\www\www83\libraries\src\Exception\ExceptionHandler.php:76)
  at Joomla\CMS\Exception\ExceptionHandler::handleException()
     (D:\www\www83\libraries\src\Application\CMSApplication.php:334)
  at Joomla\CMS\Application\CMSApplication->execute()
     (D:\www\www83\index.php:35)
[1/2] RuntimeException 
RuntimeException:
Failed to start the session because headers have already been sent by "D:\www\www83\plugins\system\debug\src\Extension\Debug.php" at line 377.

  at D:\www\www83\libraries\vendor\joomla\session\src\Storage\NativeStorage.php:454
  at Joomla\Session\Storage\NativeStorage->start()
     (D:\www\www83\libraries\src\Session\Storage\JoomlaStorage.php:313)
  at Joomla\CMS\Session\Storage\JoomlaStorage->start()
     (D:\www\www83\libraries\vendor\joomla\session\src\Session.php:396)
  at Joomla\Session\Session->start()
     (D:\www\www83\libraries\vendor\joomla\session\src\Session.php:327)
  at Joomla\Session\Session->has()
     (D:\www\www83\libraries\src\Session\Session.php:194)
  at Joomla\CMS\Session\Session->get()
     (D:\www\www83\libraries\src\Factory.php:372)
  at Joomla\CMS\Factory::getUser()
     (D:\www\www83\libraries\src\Application\SiteApplication.php:565)
  at Joomla\CMS\Application\SiteApplication->initialiseApp()
     (D:\www\www83\libraries\src\Application\SiteApplication.php:237)
  at Joomla\CMS\Application\SiteApplication->doExecute()
     (D:\www\www83\libraries\src\Application\CMSApplication.php:304)
  at Joomla\CMS\Application\CMSApplication->execute()
     (D:\www\www83\index.php:35)