ГОСТ Р ИСО 17234-2-2015 Кожа. Химические испытания для определения содержания некоторых азокрасителей в окрашенной коже. Часть 2. Метод определения содержания 4-аминоазобензола
ГОСТ Р ИСО 17234-2-2015
НАЦИОНАЛЬНЫЙ СТАНДАРТ РОССИЙСКОЙ ФЕДЕРАЦИИ
КОЖА
Химические испытания для определения содержания некоторых азокрасителей в окрашенной коже
Часть 2
Метод определения содержания 4-аминоазобензола
Leather. Chemical tests for the determination of certain azo colorants in dyed leathers. Part 2. Method for determination of 4-aminoazobenzene
ОКС 59.140.30
Дата введения 2016-07-01
Предисловие
1 ПОДГОТОВЛЕН Техническим комитетом по стандартизации ТК 412 "Текстиль", Открытым акционерным обществом "Всероссийский научно-исследовательский институт сертификации" (ОАО "ВНИИС") на основе собственного аутентичного перевода на русский язык международного стандарта, указанного в пункте 4
2 ВНЕСЕН Управлением технического регулирования и стандартизации Федерального агентства по техническому регулированию и метрологии
3 УТВЕРЖДЕН И ВВЕДЕН В ДЕЙСТВИЕ Приказом Федерального агентства по техническому регулированию и метрологии от 19 июня 2015 г. N 751-ст
4 Настоящий стандарт идентичен международному стандарту ИСО 17234-2:2011* "Кожа. Химические испытания для определения содержания некоторых азокрасителей в окрашенной коже. Часть 2. Определение содержания 4-аминоазобензола" (ISO 17234-2:2011 "Leather - Chemical tests for the determination of certain azo colorants in dyed leathers - Part 2: Determination of 4-aminoazobenzene").
________________
* Доступ к международным и зарубежным документам, упомянутым в тексте, можно получить, обратившись в Службу поддержки пользователей. - Примечание изготовителя базы данных.
Наименование настоящего стандарта изменено относительно наименования указанного международного стандарта для приведения в соответствие с ГОСТ Р 1.5 (пункт 3.5).
При применении настоящего стандарта рекомендуется использовать вместо ссылочных международных стандартов соответствующие им национальные стандарты Российской Федерации, сведения о которых приведены в дополнительном приложении ДА
5 ВВЕДЕН ВПЕРВЫЕ
Правила применения настоящего стандарта установлены в ГОСТ Р 1.0-2012 (раздел 8). Информация об изменениях к настоящему стандарту публикуется в ежегодном (по состоянию на 1 января текущего года) информационном указателе "Национальные стандарты", а официальный текст изменений и поправок - в ежемесячном информационном указателе "Национальные стандарты". В случае пересмотра (замены) или отмены настоящего стандарта соответствующее уведомление будет опубликовано в ближайшем выпуске ежемесячного информационного указателя "Национальные стандарты". Соответствующая информация, уведомление и тексты размещаются также в информационной системе общего пользования - на официальном сайте Федерального агентства по техническому регулированию и метрологии в сети Интернет (www.gost.ru)
1 Область применения
Настоящий стандарт дополняет ИСО 17234-1 и устанавливает специальный метод для определения наличия в продукции некоторых азокрасителей, способных выделять 4-аминоазобензол. Данный метод также позволяет обнаружить 4-аминоазобензол (краситель анилиновый желтый 1), уже присутствующий в качестве свободного амина в продукции, не прошедшей восстановительное расщепление.
Азокрасители, способные образовывать 4-аминоазобензол, генерируют в условиях, установленных ИСО 17234-1, для определения аминов, анилина и 1,4-фенилендиамина. Наличие красителей на основе 4-аминоазобензола невозможно надежно установить без дополнительной информации (например, химического состава использованного красителя) или без специальной методики.
Данным методом невозможно определить количественное содержание использованных азокрасителей, способных выделять в процессе восстановительного расщепления азогруппы (азогрупп) один или несколько других ароматических аминов, приведенных в приложении XVII к Регламенту EC 1907/2006 Европейского парламента и Совета о регистрации, оценке, разрешении и ограничении (запрещении) применения химических веществ [Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (Регламент REACH)], за исключением 4-аминоазобензола.
2 Нормативные ссылки
В настоящем стандарте использованы нормативные ссылки на следующие международные стандарты*:
_______________
* Таблицу соответствия национальных стандартов международным см. по ссылке. - Примечание изготовителя базы данных.
ИСО 2418:2002 Кожа. Химические, физические и механические испытания и испытания на прочность. Определение местоположения образца (ISO 2418:2002 Leather - Chemical, physical and mechanical and fastness tests - Sampling location)
ИСО 4044:2008 Кожа. Химические испытания. Подготовка образцов для химических испытаний (ISO 4044:2008 Leather - Chemical tests - Preparation of chemical test samples)
3 Общие положения
Некоторые азокрасители способны выделять при восстановительном расщеплении азогрупп(ы) вещество 4-аминоазобензол, которое запрещено согласно приложению XVII к Регламенту REACH.
Таблица 1 - 4-аминоазобензол, запрещенный Регламентом REACH 1907/2006 (приложение XVII)
N |
Номер по CAS |
Номер по указателю |
Номер в EC |
Вещество |
22 |
60-09-3 |
611-008-00-4 |
200-453-6 |
4-аминоазобензол |
4 Принцип
После обезжиривания образец кожи обрабатывают дитионитом натрия в щелочном растворе при температуре 40°C в закрытом сосуде. 4-аминоазобензол, выделяющийся в процессе восстановления, переводят в фазу трет-бутилметилового эфира с помощью экстракции в системе "жидкость - жидкость". Аликвотное количество фазы трет-бутилметилового эфира используют для анализа.
Обнаружение и определение 4-аминоазобензола выполняют методом высокоэффективной жидкостной хроматографии [ВЭЖХ (HPLC)] с использованием фотометрического детектора на диодной матрице [ФДМД (DAD)] или масс-селективного детектора [ВЭЖХ/МСД (HPLC/MSD)], методом капиллярной газовой хроматографии с помощью масс-селективного детектора [КГХ/МСД (GC/MSD)], или методом капиллярного электрофореза с помощью фотометрического детектора на диодной матрице [КЭ/ФДМД (CE/DAD)], или количественно методом тонкослойной хроматографии или высокоэффективной тонкослойной хроматографии [ТСХ, ВЭТСХ (TLC, HPTLC)].
Если 4-аминоазобензол обнаруживают одним хроматографическим методом, необходимо выполнить подтверждение, используя один или несколько альтернативных методов. Количественное определение аминов проводят методом ВЭЖХ/ФДМД.
5 Меры предосторожности
5.1 Соединения 4-аминоазобензола относят к потенциальным канцерогенам для человека.
Работы с этими веществами и их утилизацию необходимо проводить в строгом соответствии с национальными регламентами по здравоохранению и безопасности.
5.2 Пользователь несет ответственность за соблюдение безопасной и надежной техники обращения с материалами данного метода испытаний. Относительно конкретных подробностей, таких, например, как таблицы по безопасности материалов и другие рекомендации, необходимо проконсультироваться с изготовителями.
5.3 Рекомендуется следовать правилам надлежащей лабораторной практики. В любом из помещений лаборатории при работе с порошкообразными красителями и 4-аминоазобензолом необходимо пользоваться защитными очками, противопылевыми респираторами и одноразовыми перчатками.
5.4 Пользователи должны соблюдать требования национальных и местных правил техники безопасности.
6 Аппаратура
Стандартное лабораторное оборудование и, в частности, следующее.
6.1 Подходящий для реакции сосуд из термостойкого стекла с газонепроницаемой пробкой.
6.2 Нагреватель, создающий температуру (40±2)°C.
6.3 Сепаратор со скоростью вращения более 3000 об/мин.
6.4 Ротационный вакуумный испаритель.
6.5 Пипетки требуемого размера или разные.
6.6 Ультразвуковая ванна не менее 160 Вт, с регулируемым нагревом.
6.7 Горизонтальный встряхиватель с достаточной частотой 5 с
, длиной перемещения от 2 до 5 см.
6.8 Полипропиленовый или полиэтиленовый шприц объемом 2 мл.
6.9 Оборудование для следующих методов
6.9.1 Газовая хроматография (ГХ) с масс-селективным детектором (МСД).
6.9.2 Высокоэффективная жидкостная хроматография (ВЭЖХ) с градиентом элюирования и фотометрическим детектором на диодной матрице (ФДМД) или масс-селективным детектором (МСД).
6.9.3 Тонкослойная хроматография (ТСХ) или высокоэффективная тонкослойная хроматография (ВЭТСХ) с соответствующим детектированием.
6.9.4 Капиллярный электрофорез (КЭ) с детектором ФДМД.
Примечание - Описание оборудования приведено в приложении A.
7 Реактивы
Если нет иных указаний, применяют химические вещества аналитической чистоты.
7.1 Гидроксид натрия.
7.2 Водный раствор дитионита натрия, 
=200 мг/мл
, свежеприготовленный, для использования непосредственно после выдерживания в течение 1 ч в закрытом сосуде.
________________ - концентрация по массе (масса вещества на единицу массы смеси).
7.3 Раствор гидроксида натрия, w=2%.
________________ w - процентная концентрация по массе (массовая доля).
7.4 н-гексан.
7.5 трет-бутилметиловый эфир.
7.6 Хлорид натрия.
7.7 4-аминоазобензол, сверхчистый.
7.8 Внутренние стандарты для газовой хроматографии (ИС), например:
- ИС 1: нафталин-d8 (CAS No.: 1146-65-2);
- ИС 2: 2,4,5-трихлоранилин (CAS No.: 636-30-6);
- ИС 3: бензидин-d8 (CAS No.: 92890-63-6);
- ИС 4: антрацен-d10 (CAS No.: 1719-06-8).
7.9 Стандартные растворы
7.9.1 Раствор внутреннего стандарта (ИС) в трет-бутилметиловом эфире, =10,0 мкг/мл.
7.9.2 Градуировочный раствор 4-аминоазобензола для проверки методики эксперимента и приготовления градуировочных растворов 4-аминоазобензола в метаноле, =500 мкг/мл.
8 Отбор проб
Если возможно, проводят отбор проб в соответствии с ИСО 2418 и измельчают кожу в соответствии с ИСО 4044. Если отбор проб в соответствии с ИСО 2418 невозможен (например, в случае отбора кожи из готовых отделанных изделий, таких как обувь или одежда), в протоколе испытаний описывают процедуру отбора проб.
Все следы клея должны быть удалены механическим способом.
В случае кожаного лоскутного изделия с разноцветным рисунком различные цвета, по возможности, рассматривают отдельно. Для изделий, изготовленных из кожи различного качества, образцы кожи различного качества анализируют отдельно.
9 Проведение анализа
9.1 Обезжиривание
Обрабатывают кожу массой более 1,0 г, измельченную на кусочки (площадью 25 мм
), или измельченный образец кожи, помещая в закрытый сосуд вместимостью 50 мл (см. 6.1), порцией 20 мл н-гексана (см. 7.4), в ультразвуковой ванне (см. 6.6) при температуре (40±2)°C в течение 20 мин.
Декантируют слой н-гексана с образца кожи. Следует избегать потерь частиц кожи во время декантирования. Сразу после декантирования обрабатывают образец так же, как до этого, порцией 20 мл н-гексана. Выпаривают остаток н-гексана из открытого сосуда в течение ночи или более длительного срока.
9.2 Восстановительное расщепление
Добавляют 9 мл раствора гидроксида натрия (см. 7.3) к образцу. Плотно закупоривают реакционный сосуд и энергично встряхивают. Все волокна кожаного материала следует смочить.
Затем с помощью шприца (см. 6.8) добавляют 1,0 мл водного раствора дитионита натрия (см. 7.2). Образец с восстановительным раствором энергично встряхивают и выдерживают при температуре (40±2)°C в течение точного интервала времени, 30 мин. Затем охлаждают до комнатной температуры (от 20°C до 25°C) в течение 1 мин водой или, если необходимо, охлаждающей смесью льда, воды и соли.
9.3 Отделение и концентрирование 4-аминоазобензола
Добавляют 5 мл трет-бутилметилового эфира (см. 7.5) или 5 мл раствора внутреннего стандарта (см. 7.9.1) в реакционный раствор. После этого добавляют 7 г хлорида натрия (см. 7.6) и встряхивают смесь непрерывно в течение 45 мин, с частотой встряхивания f=5 с (см. 6.7). Для полного разделения фаз смесь после встряхивания центрифугируют.
Задержка между охлаждением и встряхиванием рекомендуется не более 5 мин.
Для последующего анализа переносят аликвотное количество фазы трет-бутилметилового эфира в подходящий сосуд, который немедленно закрывают. Выполняют обнаружение и определение 4-аминоазобензола хроматографическими методами, перечисленными в 6.9.
РЕКОМЕНДАЦИЯ - Для некоторых методов анализа может потребоваться концентрирование экстракта, полученного по 9.3, или перенос его в другой подходящий растворитель (например, метанол). Рекомендуется концентрировать экстрагированную фазу трет-бутилметилового эфира до примерно 1 мл (не досуха) в вакуумном ротационном испарителе при небольшом разрежении и температуре не более 50°C. Затем удалить остаток растворителя очень осторожно, без вакуума, в слабом токе инертного газа.
Примечание 1 - Удаление растворителя (концентрирование в вакуумном ротационном испарителе, выпаривание досуха) может привести к значительным потерям 4-аминоазобензола, если выполнять процедуру без контроля.
Примечание 2 - Если возможно, стараются избежать замены растворителя, поскольку в процессе анализа значительные потери анализируемого вещества могут произойти за счет матричных эффектов.
9.4 Градуировочная смесь
Добавляют 5 мл трет-бутилметилового эфира (см. 7.5) или 5 мл раствора внутреннего стандарта (см. 7.9.1) к 100 мкл градуировочного раствора 4-аминоазобензола (см. 7.9.2). Эту смесь используют для калибровки, поскольку извлечение 4-аминоазобензола при разделении фаз с использованием данной методики составляет от 95% до 100%.
9.5 Проверка аналитической системы
Чтобы проверить методику, 100 мкл градуировочного раствора 4-аминоазобензола (см. 7.9.2) обрабатывают согласно 9.2 и 9.3. Степень извлечения 4-аминоазобензола должна быть не менее 60%.
9.6 Хроматографический анализ
Обнаружение 4-аминоазобензола можно произвести с помощью хроматографических методов, перечисленных в 6.9. Можно использовать другие подтвержденные методы. Количественное определение 4-аминоазобензола выполняют с помощью метода ВЭЖХ/ФДМД или КГХ/МСД; если используют газовую хроматографию, применяют соответствующие внутренние стандарты (см. 7.8).
10 Оценка
Количество 4-аминоазобензола обычно вычисляют с помощью компьютерной программы. Расчет можно осуществить вручную по площадям пиков.
10.1 Вычисление с помощью внутреннего стандарта
Концентрацию 4-аминоазобензола, w, вычисляют как массовую долю, в миллиграммах на килограмм (мг/кг) образца, по следующей формуле:
где 
- концентрация 4-аминоазобензола в градуировочном растворе, мкг/мл;
A
- площадь пика 4-аминоазобензола в растворе образца, в единицах площади;
A
- площадь пика 4-аминоазобензола в градуировочном растворе, в единицах площади;
A
- площадь пика внутреннего стандарта в растворе образца, в единицах площади;
________________ Количественный анализ с помощью ГХ/МСД.
A
- площадь пика внутреннего стандарта в градуировочном растворе, в единицах площади;
________________ Количественный анализ с помощью ГХ/МСД.
V - объем образца согласно 9.3 (конечный объем образца), мл; здесь: 5 мл;
m
- масса образца кожи, г.
10.2 Расчет без внутреннего стандарта
Концентрацию 4-аминоазобензола вычисляют как массовую долю w, мг/кг, по следующей формуле:
где - концентрация 4-аминоазобензола в градуировочном растворе, в микрограммах на миллилитр (мкг/мл);
A - площадь пика 4-аминоазобензола в растворе образца, в единицах площади;
A - площадь пика 4-аминоазобензола в градуировочном растворе, в единицах площади;
V - объем образца согласно 9.3 (конечный объем образца), мл; здесь: 5 мл;
m - масса образца кожи, г.
10.3 Надежность метода
В отношении надежности метода см. приложение B.
11 Протокол испытания
Протокол испытания должен включать следующее:
a) ссылку на настоящий стандарт;
b) вид, происхождение и обозначение образца (составной образец, если применим);
c) дату поступления образца и дату проведения анализа;
d) процедуру отбора проб;
e) примененные методы детектирования и количественного определения;
f) результаты, сообщаемые как концентрация и предел обнаружения 4-аминоазобензола, в мг/кг. Следует быть внимательным в интерпретации результатов при получении значения 4-аминоазобензола менее 30 мг/кг (см. приложение C).
Приложение А (справочное). Методы хроматографического анализа
Приложение А
(справочное)
A.1 Предварительное замечание
Поскольку оснащение (см. 6.9) лабораторий может быть различным, для хроматографических анализов невозможно представить общие инструкции. Успешно испытываются и используются следующие параметры.
A.2 Высокоэффективная жидкостная хроматография (ВЭЖХ) (количественный метод)
A.2.1 Высокоэффективная жидкостная хроматография/фотометрический детектор с диодной матрицей (ВЭЖХ/ФДМД)
Элюент 1 |
метанол; |
||
Элюент 2 |
0,575 г дигидрофосфата аммония +0,7 г гидрофосфата натрия в 1000 мл воды, уровень pH=6,9; |
||
Неподвижная фаза |
Zorbax SB-Phenyl |
||
________________ |
|||
Скорость потока | от 0,7 до 1,0 мл/мин; |
||
Градиент | см. таблицу A.1; |
||
Таблица A.1 - Программа градиента
Время, мин |
Элюент 1, % |
Элюент 2, % |
0 |
0 |
100 |
5 |
10 |
90 |
10 |
10 |
90 |
27 |
68 |
32 |
29 |
100 |
0 |
Температура колонки |
30°C; |
|
Вводимый объем пробы |
10,0 мкл; |
|
Детектирование |
ФДМД, спектрограф; |
|
Количественный анализ |
при 240, 280, 305 и 380 нм. |
A.2.2 Высокоэффективная жидкостная хроматография/масс-селективный детектор (ВЭЖХ/ФДМД/МСД)
Элюент 1 |
ацетонитрил; |
|
Элюент 2 |
ацетат аммония в 1000 мл воды, 5 ммоль, уровень pH=3,0; |
|
Неподвижная фаза |
Zorbax Eclipse XDB C18 |
|
________________ |
||
Скорость потока |
300 мкл/мин; |
|
Градиент |
см. таблицу A.2; |
|
Таблица A.2 - Программа градиента
Время, мин |
Элюент 1, % |
Элюент 2, % |
0 |
10 |
90 |
1,5 |
20 |
80 |
7,5 |
90 |
10 |
Температура колонки |
40°C; |
|
Вводимый объем |
2,0 мкл; |
|
Обнаружение |
квадрупольная и/или масс-спектрометрическая ионная ловушка, режим сканирования и/или МС детектирование МС-дочернего иона; ФДМД: в отношении длины волны см. A.2.1; |
|
Газ-спрей |
азот (в сосудах/генераторный); |
|
Ионизация |
электрораспыление, положительное, по API, фрагментор 120 В. |
A.3 Капиллярная газовая хроматография (КГХ/МСД) (количественный метод)
Капиллярная колонка |
ZB-5-(Zebron) |
|
________________ |
||
Система ввода |
без деления; |
|
Температура инжектора |
250°C; |
|
Газ-носитель |
гелий; |
|
Температурная программа |
50°C (3 мин), от 50°C до 280°C (15°C/мин), 280°C (6 мин); |
|
Вводимый объем |
1,0 мкл, деление 1:15; |
|
Детектирование |
МС. |
|
A.4 Капиллярный электрофорез (КЭ/ФДМД) (количественный метод)
200 мкл раствора образца (см. 9.3) смешивают с 50 мкл HCl (c=0,01 моль/л) и пропускают через мембранный фильтр (0,2 мкм). Этот раствор анализируют с помощью капиллярного зонального электрофореза.
Капилляр 1 |
56 см, без покрытия, внутренний диаметр 50 мкм, с увеличенной толщиной светопоглощающего слоя; |
|
Капилляр 2 |
56 см, покрытый поливиниловым спиртом (ПВС), внутренний диаметр 50 мкм, с увеличенной толщиной светопоглощающего слоя; |
|
Буферный раствор |
фосфатный буферный раствор (c=50 ммоль/л), уровень pH=2,5; |
|
Температура колонки |
25°C; |
|
Напряжение |
30 кВ; |
|
Время ввода |
4 с; |
|
Время продувки |
5 с; |
|
Детектирование |
ФДМД 214, 254 нм, спектрограф. |
A.5 Тонкослойная хроматография (ТСХ) (количественный метод); ВЭТСХ или ТСХ только для полуколичественного подтверждения
A.5.1
Пластины (ВЭТСХ): силикагель 60 с флуоресцентным индикатором F254, (20х10) см.
Применяемый объем: (2-5) мкл, наносится в виде капли.
Подвижный растворитель 1: хлороформ/уксусная кислота (90+10) частей на объем.
A.5.2
Пластины (ТСХ): силикагель 60 с флуоресцентным индикатором F254, (20х20) см.
Применяемый объем: 10,0 мкл, наносится в виде линии.
Подвижный растворитель 2: хлороформ/этилацетат/уксусная кислота (60+30+10) частей на объем.
Подвижный растворитель 3: хлороформ/метанол (95+5) частей на объем.
Подвижные растворители 2 и 3: один за другим без просушивания пластин.
A.5.3
Детектирование: |
1) ультрафиолетовая (УФ) лампа; |
|
2) после последовательной обработки реактивами 1 и 2, время реакции приблизительно 5 мин. |
Реактив 1: 0,1% NaNO
в HCl (c=1 моль/л).
Реактив 2: 0,2% 
-нафтол в KOH (c=1 моль/л).
A.6 Примеры хроматограмм и спектров
Примеры хроматограмм и спектров показаны на рисунках A.1-A.4.
Рисунок A.1 - Хроматограмма общего ионного тока, 4-аминоазобензол, КГХ/МСД
X - время; Y - относительные единицы; 1 - внутренний стандарт; 2 - 4-аминоазобензол
Рисунок A.1 - Хроматограмма общего ионного тока, 4-аминоазобензол, КГХ/МСД
Рисунок A.2 - КГХ/МСД 70 эВ-спектр и структура 4-аминоазобензола
X - m/z; Y - относительные единицы
Рисунок A.2 - КГХ/МСД 70 эВ-спектр и структура 4-аминоазобензола
Рисунок A.3 - Хроматограмма 4-аминоазобензола, ВЭЖХ/ФДМД; детектирование при 240 и 380 нм
X - мин;
Y - мЕОП (0,001 единицы оптической плотности); 1 - ФДМД A, сигнал =240; 2 - 4-аминоазобензол; 3 - ФДМД B, сигнал=380
Рисунок A.3 - Хроматограмма 4-аминоазобензола, ВЭЖХ/ФДМД; детектирование при 240 и 380 нм
Рисунок A.4 - ВЭЖХ/ФДМД-спектр 4-аминоазобензола
X - нм; Y - мЕОП (0,001 единицы оптической плотности)
Рисунок A.4 - ВЭЖХ/ФДМД-спектр 4-аминоазобензола
Приложение B (справочное). Надежность метода
Приложение B
(справочное)
Таблица B.1 касается межлабораторных испытаний, выполненных для определения содержания 4-аминоазобензола в коже
Таблица B.1 - Результаты межлабораторных испытаний. Определение концентрации образовавшегося 4-аминоазобензола в коже [1]
Параметр | Методика анализа |
|
КГХ/МСД |
ВЭЖХ |
|
Число лабораторий-участниц |
10 |
11 |
Число выбросов |
2 |
2 |
Число лабораторий после исключения выбросов |
8 |
9 |
Среднее значение x, мг/кг |
81,9 |
91,2 |
Повторяемость r, мг/кг |
21,4 |
27,1 |
Стандартное отклонение повторяемости s |
7,6 |
9,7 |
Воспроизводимость R, мг/кг |
32,5 |
35,9 |
Стандартное отклонение воспроизводимости s |
11,6 |
12,5 |
, мг/кг
, мг/кг
Данный официальный метод был разработан рабочей группой "Анализ запрещенных азокрасителей" германской BVL и оценен в межлабораторном испытании, в котором приняли участие 11 лабораторий.
a) В отношении оценки повторяемости и воспроизводимости результатов межлабораторных испытаний (по круговой схеме) необходимо учесть следующее:
1) межлабораторные испытания продемонстрировали, что отношение красителя к восстановителю и "возраст" восстановителя могут оказывать решающее влияние на количественный результат. Следовательно, рекомендуется выполнять восстановительное расщепление в строгом соответствии с условиями, изложенными в 9.2 (время, температура и количество);
2) другим важным фактором является экстракция системы "жидкость - жидкость", например, разделение водной и органической фаз, чтобы предотвратить дальнейшую реакцию расщепления азогруппы 4-аминоазобензола. Следовательно, настоятельно рекомендуется точно соблюдать условия, изложенные в 9.3.
b) Пробу кожи для межлабораторных испытаний взяли от типового изделия, разрезали и смешали с неокрашенной кожей. Таким образом можно снизить гомогенность материала.
c) Применение других подходящих внутренних стандартов может привести к более высокой повторяемости метода КГХ/МСД. Это условие, однако, не рассматривалось в оценке межлабораторных испытаний.
Приложение C (справочное). Руководство по оценке. Интерпретация результатов анализа
Приложение C
(справочное)
Поскольку получение аминов в очень небольших количествах может привести к ложным положительным результатам, приложение XVII Регламента REACH 1907/2006 определяет предельное значение как 30 мг/кг материала пробы. Это значение применяется только в пробе материала, который является гомогенным по структуре и окрашиванию, а не к смешанной пробе гетерогенного состава.
Если обнаруженное количество 4-аминоазобензола превышает 30 мг/кг, можно предположить, что был использован определенный азокраситель. При концентрации ниже 30 мг/кг в настоящее время невозможно сделать авторитетное заявление об использовании определенных азокрасителей без получения дополнительной информации, такой, например, как тип и/или чистота использованных красителей или другого использованного сырья.
В этом контексте рекомендуется сообщать результаты анализа следующим образом:
В случае, когда концентрация образовавшегося 4-аминоазобензола не более 30 мг/кг:
"Согласно выполненному анализу азокрасителей, способных выделять 4-аминоазобензол в результате восстановительного расщепления их азогрупп(ы), в предложенном изделии обнаружено не было".
В случае, когда концентрация образовавшегося 4-аминоазобензола более 30 мг/кг:
"Согласно выполненному анализу предполагается, что предложенное изделие изготовлено или обработано с применением азокрасителей, запрещенных в соответствии с приложением XVII Регламента REACH 1907/2006".
Приложение ДА (справочное). Сведения о соответствии ссылочных международных стандартов национальным стандартам Российской Федерации
Приложение ДА
(справочное)
Таблица ДА.1
Обозначение ссылочного международного стандарта |
Степень соответствия |
Обозначение и наименование соответствующего национального стандарта |
ИСО 2418:2002 |
- |
* |
ИСO 4044:2008 |
- |
* |
* Соответствующий национальный стандарт отсутствует. До его утверждения рекомендуется использовать перевод на русский язык данного международного стандарта. Перевод данного международного стандарта находится в Федеральном информационном фонде технических регламентов и стандартов. |
||
Библиография
[1] |
Amtliche Sammlung von Untersuchungsverfahren nach § 64 LFGB B 82.02-9:2006-09/BVL B 82.02-9:2006-09 Berichtigung 2008-04 - Nachweis der Verwendung von Azofarbstoffen, die 4-Aminoazobenzol freisetzen |
[2] |
Регламент REACH: Regulation (EC) No. 1907/2006 of the European Parliament and of the Council concerning the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH), Annex XVII |
УДК 675.046.12:006.354 |
ОКС 59.140.30 |
|
Ключевые слова: окрашенная кожа, азокраситель, 4-аминоазобензол, определение, принцип, процедура, оценка, протокол |
||
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